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

HRID 1041915노트

반응식

HRID 1041915 반응식
[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

참가 물질

6

반응물 4

HCID 6344Dichloromethane2회HCID 7656DibenzylamineHCID 8471TriethylamineHCID 203124,6-Dichloro-5-nitropyrimidine

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e7e77e3a67504ea2addbe56e56e5f2cd
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557803B2

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