Potassium Hydroxide → HCID 178473885、化合物

HRID 645679ノート

反応式

HRID 645679 の反応式
[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([NH:11][C:12]3[C:13]4[CH:36]=[CH:35][N:34](S(C5C=CC(C)=CC=5)(=O)=O)[C:14]=4[N:15]=[C:16]([NH:18][C:19]4[CH:24]=[CH:23][C:22]([N:25]5[CH2:30][CH2:29][N:28]([C:31](=[O:33])[CH3:32])[CH2:27][CH2:26]5)=[CH:21][CH:20]=4)[N:17]=3)=[CH:8][CH:9]=2)[NH:4][N:3]=1.[OH-].[K+]>CO>[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([NH:11][C:12]3[C:13]4[CH:36]=[CH:35][NH:34][C:14]=4[N:15]=[C:16]([NH:18][C:19]4[CH:24]=[CH:23][C:22]([N:25]5[CH2:26][CH2:27][N:28]([C:31](=[O:33])[CH3:32])[CH2:29][CH2:30]5)=[CH:21][CH:20]=4)[N:17]=3)=[CH:8][CH:9]=2)[NH:4][N:3]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 178473886HCID 178473886、化合物

生成物 1

HCID 178473885HCID 178473885、化合物収率 44.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of 1-(4-(4-(4-(3-methyl-1H-indazol-6-ylamino)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone (30 mg, 0.047 mmol) in methanol (MeOH) (3 mL), aq. 1N KOH (1.0 mL, 1.0 mmol) was added. The mixture was heated at 60° C. for 5 h. and then concentrated in vacuo. The residue was acidified with HOAc (1 mL) before being purified by HPLC to give 1-(4-(4-(4-(3-methyl-1H-indazol-6-ylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone (10 mg), MS 482.2 (M+H) (Compound 2-1); and N4-(3-methyl-1H-indazol-6-yl)-N2-(4-(piperazin-1-yl)phenyl)-7H-pyrrolo[2,3-d]pyrimidine-2,4-diamine (3 mg), MS 440.1 (M+H) (Compound 2-2).

後処理

  1. concentrationconcentrated in vacuo
  2. custombefore being purified by HPLC

出典と根拠

ORDレコード
ord-548100623a924643ba749ba85117972f
出典データセット
uspto-grants-2010_04
特許番号
US07705004B2

反応ノート

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