Methanol → N-benzyl-6-chloropyrimidin-4-amine

HRID 1886815노트

반응식

HRID 1886815 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:15]=[C:14](Cl)[N:13]=[CH:12][N:11]=1.C(N(CC)CC)C.CO>C(Cl)Cl>[CH2:1]([NH:8][C:14]1[CH:15]=[C:10]([Cl:9])[N:11]=[CH:12][N:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 7504BenzylamineHCID 8471TriethylamineHCID 709434,6-Dichloropyrimidine

생성물 1

HCID 3771857N-benzyl-6-chloropyrimidin-4-amine수율 79%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Benzyl amine (0.697 ml, 6.76 mmol) was added to 4,6-dichloropyrimidine (1.0 g, 6.76 mmol) neat causing a vigorous reaction and color change. The reaction was slowly diluted with methylene chloride resulting in a white precipitate. 1 ml of triethyl amine was added and TLC indicated conversion to product (5% MeOH:methylene chloride). The reaction was loaded directly onto a silica and purified (eluent:2% MeOH:methylene chloride) giving 1.17 g (5.32 mmol) of 12 as a yellow wax in 79% yield.

후처리

  1. customa vigorous reaction and color change
  2. custompurified (eluent:2% MeOH:methylene chloride)

출처 및 근거

ORD 기록
ord-801bf0cf300a4c1fbdaba2f32cd8c03a
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501446B2

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