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

HRID 1041915ノート

反応式

HRID 1041915 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-e7e77e3a67504ea2addbe56e56e5f2cd
出典データセット
uspto-grants-2013_10
特許番号
US08557803B2

反応ノート

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