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

HRID 1704681노트

반응식

HRID 1704681 반응식
[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

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 20394044HCID 20394044, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
35 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-130b0b119e1745cda68804c481d62ecc
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04127606

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