Water → HCID 71534185, 화합물

HRID 1409996

반응식

HRID 1409996 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[N:10]=[CH:9][S:8][C:6]=2[N:7]=1.[CH3:12][O:13][C:14]1[CH:15]=[C:16]([NH2:22])[CH:17]=[CH:18][C:19]=1[O:20][CH3:21].CCN(C(C)C)C(C)C.O>CS(C)=O>[Cl:1][C:2]1[N:3]=[C:4]([NH:22][C:16]2[CH:17]=[CH:18][C:19]([O:20][CH3:21])=[C:14]([O:13][CH3:12])[CH:15]=2)[C:5]2[N:10]=[CH:9][S:8][C:6]=2[N:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 227703,4-DimethoxyanilineHCID 81531DiisopropylethylamineHCID 6096395,7-Dichlorothiazolo(5,4-d)pyrimidine

생성물 1

HCID 71534185HCID 71534185, 화합물수율 63.8%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 5,7-dichloro-thiazolo[5,4-d]pyrimidine (0.925 g, 4.49 mmol), 3,4-dimethoxy-phenylamine (0.89 g, 5.83 mmol) and DIEA (0.86 g, 6.73 mmol) in 12 mL of DMSO was stirred at room temperature for two hours. The mixture was poured into 50 mL of water and filtered; the solid obtained was washed with water (50 mL) to give a crude product. It was purified by silica gel chromatography (silica gel 200-300 mesh, ethyl acetate as eluent) to give (5-chloro-thiazolo[5,4-d]pyrimidin-7-yl)-(3,4-dimethoxy-phenyl)-amine (0.92 g, 63.8%) as a solid. LC-MS: 323.1 [M+H]+, tR=1.56 min.

후처리

  1. filtrationfiltered
  2. customthe solid obtained
  3. washwas washed with water (50 mL)
  4. customto give a crude product
  5. customIt was purified by silica gel chromatography (silica gel 200-300 mesh, ethyl acetate as eluent)

출처 및 근거

ORD 기록
ord-2f4bc905bf85461abd0aa70a2b3a5c49
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921383B2

연결된 노트

불러오는 중…