Water → HCID 71534185、化合物

HRID 1410093

反応式

HRID 1410093 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 82.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 5,7-dichlorothiazolo[5,4-d]pyrimidine (0.925 g, 4.49 mmol), 3,4-dimethoxybenzenamine (0.89 g, 5.8 mmol) and DIEA (0.86 g, 6.66 mmol) in 12 mL of DMSO was stirred at room temperature for 24 hours. Then the reaction mixture was poured into 50 mL of water, the solid was filtered and washed with water (50 mL) to give a crude product as a solid. It was purified by silica gel chromatography (silica gel 200-300 mesh, eluting with ethyl acetate) to give 5-chloro-N-(3,4-dimethoxyphenyl)thiazolo[5,4-d]pyrimidin-7-amine (1.2 g, 82.8%) as a grey solid. LC-MS: 322.9 [M+H]+, tR=1.51 min.

後処理

  1. filtrationthe solid was filtered
  2. washwashed with water (50 mL)
  3. customto give a crude product as a solid
  4. customIt was purified by silica gel chromatography (silica gel 200-300 mesh, eluting with ethyl acetate)

出典と根拠

ORDレコード
ord-45b3fadfb00d4288b0af4ae254ea6cdf
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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