1-p-Fluorobenzyl-2-nitromethylene-pyrrolidine → 2-Aminomethyl-1-p-fluorobenzyl-pyrrolidine

HRID 426953

반응식

HRID 426953 반응식
[F:1][C:2]1[CH:17]=[CH:16][C:5]([CH2:6][N:7]2[CH2:11][CH2:10][CH2:9][C:8]2=[CH:12][N+:13]([O-])=O)=[CH:4][CH:3]=1>CO.[Ni]>[NH2:13][CH2:12][CH:8]1[CH2:9][CH2:10][CH2:11][N:7]1[CH2:6][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:17][CH:16]=1

참가 물질

4

반응물 1

HCID 540091111-p-Fluorobenzyl-2-nitromethylene-pyrrolidine

생성물 1

HCID 147090372-Aminomethyl-1-p-fluorobenzyl-pyrrolidine수율 72.4%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

A solution of 27 g (0.114 mol) of 1-p-fluorobenzyl-2-nitromethylene-pyrrolidine in 600 ml of methanol is hydrogenated at ambient temperature and atmospheric pressure in the presence of Raney nickel. When the theoretical amount of hydrogen has been absorbed, which requires about one hour, the catalyst is filtered off and the methanol is evaporated from the filtrate. The product which remains is distilled under reduced pressure. 17.2 g (yield: 72%) of 2-aminomethyl-1-p-fluorobenzyl-pyrrolidine are collected as a colourless liquid distilling at 80°-82° under a pressure of 0.01 mm of mercury; this product is used, without further purification, in the next stage of the synthesis.

후처리

  1. customis hydrogenated at ambient temperature
  2. customWhen the theoretical amount of hydrogen has been absorbed
  3. filtrationthe catalyst is filtered off
  4. customthe methanol is evaporated from the filtrate
  5. distillationThe product which remains is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-8f6fffddd1ce4182836eaaece3ed2e1c
출처 데이터셋
uspto-grants-1979_10
특허 번호
US04172143

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