Methyl acetoacetate → HCID 70611054, 화합물

HRID 1678877노트

반응식

HRID 1678877 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; 38.4 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 evaporated 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. customthe solvent was evaporated in vacuo
  7. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-69383cba832e4e17854012455eae56bf
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04077976

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