Water → HCID 71534185、化合物

HRID 1409996

反応式

HRID 1409996 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 71534185HCID 71534185、化合物収率 63.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2f4bc905bf85461abd0aa70a2b3a5c49
出典データセット
uspto-grants-2014_12
特許番号
US08921383B2

関連ノート

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