Dichloromethane → N,N-dibenzyl-6-chloro-5-nitropyrimidin-4-amine

HRID 1429341

反応式

HRID 1429341 の反応式
[CH2:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClCCl.[Cl:19][C:20]1[C:25]([N+:26]([O-:28])=[O:27])=[C:24](Cl)[N:23]=[CH:22][N:21]=1.C(N(CC)CC)C>O>[CH2:9]([N:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:24]1[C:25]([N+:26]([O-:28])=[O:27])=[C:20]([Cl:19])[N:21]=[CH:22][N:23]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 7656DibenzylamineHCID 8471TriethylamineHCID 203124,6-Dichloro-5-nitropyrimidine

生成物 1

HCID 23477266N,N-dibenzyl-6-chloro-5-nitropyrimidin-4-amine収率 105%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Dibenzylamine (10.2 g) in a dichloromethane (30 mL) solution was added dropwise on an ice bath to a dichloromethane (70 mL) solution of 4,6-dichloro-5-nitropyrimidine (10 g). This was followed by the addition of triethylamine (14.4 mL) and stirring for 1 hour. Water was then added to the reaction mixture and the organic layer was subsequently washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was concentrated under reduced pressure to obtain the title compound (19.2 g) having the physical property value indicated below.

後処理

  1. washthe organic layer was subsequently washed with saturated aqueous sodium chloride solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationThe solvent was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-002e45b3a0ba4d799633da1775f3aba8
出典データセット
uspto-grants-2015_01
特許番号
US08940725B2

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