Sodium borohydride → N-[[2-[3-(Dimethylamino)propoxy]phenyl]methyl]benzeneethanamine

HRID 1112435ノート

反応式

HRID 1112435 の反応式
[CH3:1][N:2]([CH3:23])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH:13]=[N:14][CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[BH4-].[Na+]>CO>[CH3:23][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][NH:14][CH2:15][CH2:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 20394044HCID 20394044、化合物

生成物 1

HCID 21322747N-[[2-[3-(Dimethylamino)propoxy]phenyl]methyl]benzeneethanamine収率 93.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
35 °C

実験手順

A stirred solution of 36.0 g of N-[[2-[3-(dimethylamino)propoxy]phenyl]methylene]benzeneethanamine in 200 ml of methanol is treated portionwise with 13.0 g of sodium borohydride. The temperature is maintained at 35° C using a cold water bath. After 3 hours, the solvent is evaporated and the semi-solid residue is treated with 300 ml of water. The product is extracted twice with 100 ml portions of ether. The solvent fractions are combined, treated with water, dried and concentrated to give 33.8 g of an oily product. Distillation yields 19.9 g of the title compound, boiling point 165°-170° C at 0.15 mm of Hg.

後処理

  1. customthe solvent is evaporated
  2. additionthe semi-solid residue is treated with 300 ml of water
  3. extractionThe product is extracted twice with 100 ml portions of ether
  4. additiontreated with water
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-7bfd83e1efde47b8898d895d65ce4a96
出典データセット
uspto-grants-1978_10
特許番号
US04122255

反応ノート

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