• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 引用文献
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  • 优先权
    • 专利摘要:
    1497986 Preparation of N,N-diethyl 2-(α- naphthoxy)propionamide STAUFFER CHEMICAL CO 6 Aug 1976 [15 Aug 1975] 32813/76 Heading C2C The invention comprises a process for the preparation of N,N-diethyl 2-(α-naphthoxy)- propionamide by reacting α-naphthal with an excess of N,N-diethyl α-chloro (or α-bromo)- propionamide in the presence of an excess of aqueous alkali metal hydroxide solution based on the α-naphthol and removing unreacted amide from the product.
    公开号:SU728714A3
    申请号:SU762388416
    申请日:1976-08-13
    公开日:1980-04-15
    发明作者:Михайловски Александр；Аугустус Саймон Рэймонд
    申请人:Стауффер Кемикал Компани (Фирма)；
    IPC主号:
    专利说明:

    to her 400 ml of water having the same temperature. The aqueous phase is separated, the organic phase is heated to add 200 cm of a 25% sodium hydroxide solution and 200 cm of hot water, after which the phases are separated.
    The solvent is evaporated first on a rotary evaporator under vacuum at 80 ° C and then under high vacuum (22 mm Hg) at 75 s for 2 h. The liquid product is cooled until it hardens, after which it is ground into fine powder.
    This gives 543 g of the product of 94.9% purity. Output 95% of theoretical. Melting point 12-12 ° C in the case of Technical Product and in the case of pure compound.
    Example 2. Similar to the method described in Example 1, 35.2 g (0.245 mol) of ei-naphthol, 48 g (0.3 mol) of a 25% aqueous solution of sodium hydroxide and 42.5 g (0 , 2 mol) N, N-diethylamide a-chloropropionic acid in 50 ml of toluene
    Such a solution is heated to deflation, which lasts for several hours. The reaction mixture was cooled to room temperature and washed successively with water, toluene, 25% sodium hydroxide solution and again with water. The solvent is evaporated and the hydrochloric products are cooled until solid. The yield of the target product is 89.2%; purity 93.9%.
    Example 3. 73.6 g (0.5 mol) (x.-naphthol, 47 g (0.6 mol) of 1.2% aqueous sodium hydroxide solution and 91.3 g (0.525 mol A) N, N-diethylamide ob-chloropropionic acid in 100 ml of toluene. The reflux temperature is initially 99 ° C and then decreases to 96 C. The products are treated mainly as in Example 1. The yield of the desired product is 93.6% with purity 97.2%.
    Example 4, Materials, injected into the flask, be the same as
    in example 3, but 104 g (0.6 mol) of L |, L — diethlaglide of gchloropropionic acid was used. The temperature of reflux is initially maintained at 100 ° C, but later reduced to 9 ° C.
    The output of the target dun.; a 96, with a purity of 97.8%,
    Example 5. Сm1; willow 10T: 73.6 g (Of 5 mol) of c6-naphthol, 42.9 g (0.55 mol) of 51, an aqueous solution of sodium hydroelectric hydroxide, and 95.6 g (0.55 mol) of M, H-datylate Ls. Cij-chloropropionic acid at, later the temperature decreases to 97 ° C. The yield of the desired product is 91.4% with
    S purity of 97.3%.
    At capacity 6, 73.6 g (0.5 mol) o - naphthol, 52.6 g (Of 5 mol) N, N-diethyl Hg a ;.- chloropropionic acid: 100 MO of toluene are mixed.
    Q The temperature of reflux distilled about 98 ° C. The yield of the desired product is 92.7% with a purity of 97.8%.
    Thus, the proposed method for the preparation of L, L-diethylamides of 2- (c6-5 naphthoxy) - propanoic acid allows to increase the yield and purity of the Target Product.
    Formula to the master of the game
    The method of preparation of K, dithyl-amide 2- (o (naftoksk) -propionic acid in 3 ami mode and from this and that, d - n aftolac N, N - IH ethyl Ido and ..- hapoietic acid in pr; .- 1 the presence of a silk agent and an organic solvent, o:; l and h and 1 d, and so that, in order to increase the yield and purity of the target product, an aqueous solution of hydroxide is used as an alkaline agent sodium 5, - toluene is used as a solvent and the progress is carried out at a temperature of SO-99 C to the molar ratio of the reactants: ct - n 3. ftol; N f N - in i: 3 t and l and m d at, g a loid ropionovoy acid: sodium hydroxide 1: 1,05--1 f 2; 1,05-1, 6.
    Information sources. taken into consideration r (during the experiment
    I. US patent 3480671, class, 260-559, published, 1569 (prototype
    权利要求:
    Claims (2)
    [1]
    Claim
    The method of obtaining N, N-diethylamide.
    [2]
    2- (<£ -naphthoxy) -propionic acid by reaction with £ -naphthol with Ν, Ν-diethylamide with 0-hapoid propisnic acid in the presence of a fine agent
    - and an organic solvent, which consists in the fact that in order to increase the yield and purity of the target product, a 25-50% aqueous solution of sodium hydroxide is used as an alkaline agent, toluene is used as a solvent, and the process is carried out at a temperature 90-99 ° C and a molar ratio of reactants: ct-naphthol: N, N-dithylamide /, - halopropionic acid: sodium hydroxide J = 1: 1.05-1.2: 1.05-1.6.
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    同族专利:
    公开号 | 公开日
    ZA764890B|1977-07-27|
    PH11705A|1978-05-24|
    FR2320935A1|1977-03-11|
    DE2636384C2|1986-03-06|
    IT1062668B|1984-10-20|
    BE845098A|1977-02-11|
    YU195476A|1982-02-28|
    IL50253A|1979-03-12|
    US3998880A|1976-12-21|
    IL50253D0|1976-10-31|
    BG28846A3|1980-07-15|
    ES450688A1|1977-08-01|
    GB1497986A|1978-01-12|
    MY7800485A|1978-12-31|
    DK366776A|1977-02-16|
    AU498303B2|1979-03-01|
    CA1059146A|1979-07-24|
    CS196316B2|1980-03-31|
    DE2636384A1|1977-02-24|
    NL7609044A|1977-02-17|
    HU174832B|1980-03-28|
    DK148116B|1985-03-11|
    FR2320935B1|1979-09-14|
    PL107413B1|1980-02-29|
    JPS5223056A|1977-02-21|
    DD126264A5|1977-07-06|
    AU1643076A|1978-02-02|
    JPS5711311B2|1982-03-03|
    DK148116C|1985-10-21|
    CH620669A5|1980-12-15|
    BR7605263A|1977-08-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3010996A|1961-11-28|Aryloxy acetic acid amides |
    US3007962A|1958-04-28|1961-11-07|Rhone Poulenc Sa|2-alkoxymethyl-4-chlorophenoxy-acetates|
    ES251290A1|1958-08-21|1960-04-01|Parke Davis & Co|1- pyrrolidine|
    US3213140A|1960-09-06|1965-10-19|Lilly Co Eli|2-phenyl-4, 6-dichlorophenoxyethylamine and salts thereof|
    CH432495A|1964-02-04|1967-03-31|Geigy Ag J R|Process for the preparation of new aryloxyacetic acid amides|
    FR4433M|1964-02-17|
    US3446811A|1965-04-23|1969-05-27|Parke Davis & Co|2-phenoxy-2-phenyl acetamides|
    US3480671A|1969-01-16|1969-11-25|Stauffer Chemical Co|Alpha-naphthoxy acetamide compositions|FR2398720B1|1977-07-28|1983-12-23|Rolland Sa A|
    JPH031521B2|1982-10-13|1991-01-10|Yamatake Honeywell Co Ltd|
    US4548641A|1982-11-15|1985-10-22|Stauffer Chemical Company|Herbicides: N,N-dialkyl-2- propionamides|
    KR20120055724A|2007-05-04|2012-05-31|유나이티드 포스포러스 리미티드|PROCESS FOR MANUFACTURE OF HIGH PURITY D--N, N-DIETHYL-2- PROPIONAMIDE|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/604,968|US3998880A|1975-08-15|1975-08-15|Production of N,N-diethyl 2propionamide|
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