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

HRID 236865

反応式

HRID 236865 の反応式
[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

参加物

4

反応物 1

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

生成物 1

HCID 147090372-Aminomethyl-1-p-fluorobenzyl-pyrrolidine収率 72.4%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5940074a5b9d43528d376418f1a63612
出典データセット
uspto-grants-1979_06
特許番号
US04158060

関連ノート

読み込み中…