N-Iodosuccinimide → HCID 178493476、化合物

HRID 1778650ノート

反応式

HRID 1778650 の反応式
[I:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[C:15]([O:16][CH3:17])=[CH:14][C:13]([O:18][CH3:19])=[C:12]([Cl:20])[C:11]=1[C:21]1[N:26]=[C:25]2[NH:27][N:28]=[CH:29][C:24]2=[CH:23][N:22]=1>CN(C)C=O.O>[Cl:9][C:10]1[C:15]([O:16][CH3:17])=[CH:14][C:13]([O:18][CH3:19])=[C:12]([Cl:20])[C:11]=1[C:21]1[N:26]=[C:25]2[NH:27][N:28]=[C:29]([I:1])[C:24]2=[CH:23][N:22]=1

参加物

5

反応物 2

HCID 120273N-IodosuccinimideHCID 867228036-(2,6-dichloro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidine

生成物 1

HCID 178493476HCID 178493476、化合物収率 79.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

N-Iodosuccinimide (0.23 g, 1.0 mmol) was added to a solution of 6-(2,6-dichloro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidine (0.30 g) in N,N-dimethylformamide (5.0 mL). The reaction mixture was stirred at 40° C. overnight. The reaction mixture was diluted with water and quenched with aqueous Na2S2O3. The precipitates formed were filtered, washed with water, ether, and dried in vacuum to afford the desired product (0.33 g). LCMS (M+H)+=450.8/452.8.

後処理

  1. customquenched with aqueous Na2S2O3
  2. customThe precipitates formed
  3. filtrationwere filtered
  4. washwashed with water, ether
  5. customdried in vacuum

出典と根拠

ORDレコード
ord-ec9633839d0b4a10960612dc61716fcc
出典データセット
uspto-grants-2016_02
特許番号
US09266892B2

反応ノート

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