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

HRID 1497998ノート

反応式

HRID 1497998 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.[Cl:16][C:17]1[C:22]([N+:23]([O-:25])=[O:24])=[C:21](Cl)[N:20]=[CH:19][N:18]=1.C(N(CC)CC)C.O>ClCCl>[CH2:9]([N:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:21]1[C:22]([N+:23]([O-:25])=[O:24])=[C:17]([Cl:16])[N:18]=[CH:19][N:20]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 962WaterHCID 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 6344Dichloromethane溶媒2 回

実験手順

A solution of dibenzylamine (10.2 g) in dichloromethane (30 mL) was dripped into a solution of 4,6-dichloro-5-nitropyrimidine (10 g) in dichloromethane (70 mL) on an ice bath. Then triethylamine (14.4 mL) was added, and the mixture was stirred for 1 hour. Water was added to the reaction mixture, the organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate, and the solvent was concentrated under reduced pressure to obtain the title compound (19.2 g) with the physical property value shown below.

後処理

  1. washthe organic layer was washed with a 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-80a5aff0fd7441ccbf318f407ae418f3
出典データセット
uspto-grants-2015_12
特許番号
US09199997B2

反応ノート

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