Methyl acetoacetate → HCID 70611054、化合物

HRID 1678877ノート

反応式

HRID 1678877 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 70611054HCID 70611054、化合物収率 81.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-69383cba832e4e17854012455eae56bf
出典データセット
uspto-grants-1978_03
特許番号
US04077976

反応ノート

読み込み中…