4-(Chloromethyl)-2-nitroanisole → N,N-dimethyl-N-(3-nitro-4-methoxybenzyl)-N-2-formamidoethylammonium chloride

HRID 1706104ノート

反応式

HRID 1706104 の反応式
[CH3:1][N:2]([CH3:8])[CH2:3][CH2:4][NH:5][CH:6]=[O:7].[CH3:9][O:10][C:11]1[CH:18]=[CH:17][C:14]([CH2:15][Cl:16])=[CH:13][C:12]=1[N+:19]([O-:21])=[O:20]>O>[Cl-:16].[CH3:1][N+:2]([CH3:8])([CH2:15][C:14]1[CH:17]=[CH:18][C:11]([O:10][CH3:9])=[C:12]([N+:19]([O-:21])=[O:20])[CH:13]=1)[CH2:3][CH2:4][NH:5][CH:6]=[O:7]

参加物

4

反応物 2

HCID 807854-(Chloromethyl)-2-nitroanisoleHCID 245580N-(2-(Dimethylamino)ethyl)formamide

生成物 1

HCID 86733012N,N-dimethyl-N-(3-nitro-4-methoxybenzyl)-N-2-formamidoethylammonium chloride

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A stirred solution of 24.6 parts of N-(2-dimethylaminoethyl)formamide and 30 parts of water was heated to 60° and over a period of one hour there was added 40.3 parts of 4-methoxy-3-nitrobenzylchloride. Heating between 60° and 65° C. was continued for three and one-half hours at which time the pH of the mixture stabilized above 7.0. To the cooled mixture was added 20 parts of water and the resulting mixture was clarified by filtration. An aqueous solution of N,N-dimethyl-N-(3-nitro-4-methoxybenzyl)-N-2-formamidoethylammonium chloride was obtained. This solution was used directly for reduction of the nitro group.

後処理

  1. temperatureHeating between 60° and 65° C.
  2. filtrationthe resulting mixture was clarified by filtration

出典と根拠

ORDレコード
ord-6436820296a84836992b0e29e6eff233
出典データセット
uspto-grants-1980_06
特許番号
US04206144

反応ノート

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