Methanol → HCID 834084、化合物

HRID 1153966ノート

反応式

HRID 1153966 の反応式
CO.[BH4-].[Na+].[CH:5]1([N:10]=[CH:11][C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:9][CH2:8][CH2:7][CH2:6]1.O>C(Cl)Cl>[F:18][C:15]1[CH:14]=[CH:13][C:12]([CH2:11][NH:10][CH:5]2[CH2:9][CH2:8][CH2:7][CH2:6]2)=[CH:17][CH:16]=1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 4311764Sodium borohydrideHCID 13201287HCID 13201287、化合物

生成物 1

HCID 834084HCID 834084、化合物収率 93.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

160 ml of methanol are added to 18.2 g of sodium borohydride. 90.7 g of 4-fluorobenzaldehyde-cyclopentylimide are added dropwise at 10°-15° C., while cooling with ice and stirring, and the mixture was then stirred for 1.5 hours at room temperature. 120 ml of H2O and 150 ml of methylene chloride were then added, the methylene chloride phase was separated off, and the aqueous phase was further extracted twice with CH2Cl2. The combined methylene chloride phases were washed with water and dried with Na2SO4, and the solvent was stripped off in vacuo. Distillation of the residue under a medium vacuum gave 85.9 g of N-4-fluorobenzyl-N-cyclopentylamine of boiling point 106° C. 0.25 bar.

後処理

  1. temperaturewhile cooling with ice
  2. stirringthe mixture was then stirred for 1.5 hours at room temperature
  3. customthe methylene chloride phase was separated off
  4. extractionthe aqueous phase was further extracted twice with CH2Cl2
  5. washThe combined methylene chloride phases were washed with water
  6. dry with materialdried with Na2SO4
  7. distillationDistillation of the residue under a medium vacuum

出典と根拠

ORDレコード
ord-9688974949384867b5dbbc553983ca80
出典データセット
uspto-grants-1984_12
特許番号
US04487783

反応ノート

読み込み中…