Methyl acetoacetate → HCID 70611054, 화합물

HRID 261455노트

반응식

HRID 261455 반응식
[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][NH2:9])[CH3:2].[2H]Cl.[C:12]([O:18][CH3:19])(=[O:17])[CH2:13][C:14]([CH3:16])=O.S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][NH:9]/[C:14](/[CH3:16])=[CH:13]\[C:12]([O:18][CH3:19])=[O:17])[CH3:2]

참가 물질

6

반응물 4

HCID 7757Methyl acetoacetateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 522634Deuterium chloride

생성물 1

HCID 70611054HCID 70611054, 화합물수율 81.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

38.4 G (0.3 MOLE) OF N-ethyl-2-aminomethylpyrrolidine and a drop of hydrochloric acid d=1.18 were added into a 250 ml flask provided with a stirrer, a thermometer, a condenser and a dropping funnel; 34.8 g (0.3 mole) of methyl acetoacetate were added drop by drop. The temperature reached 54° C. by the end of the introduction. The mixture was next allowed to return to ambient temperature while stirring, and 150 ml of methylene chloride and 5 g of magnesium sulphate were then added. The mixture was stirred for one hour, filtered, the solvent was vaporated in vacuo, and the residue was distilled. 55 g of methyl N-(1-ethyl-2-pyrrolidylmethyl)-3-aminocrotonate were obtained. (Yield: 81.1%; boiling point--3 mm/Hg: 132°-134° C.).

후처리

  1. customprovided with a stirrer
  2. customreached 54° C. by the end of the introduction
  3. customto return to ambient temperature
  4. stirringThe mixture was stirred for one hour
  5. filtrationfiltered
  6. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-09a72ade9e7545d9a6f1dffaae447e9f
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166060

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