Dimethylamine → HCID 44539633、化合物

HRID 1616028ノート

反応式

HRID 1616028 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:10][C:11]2[CH:19]=[C:18]([C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[CH:17]=[C:16]3[C:12]=2[CH:13]=[N:14][NH:15]3)=[O:9])[C:5](F)=[CH:4][CH:3]=1.[CH3:30][NH:31][CH3:32].CCN(C(C)C)C(C)C>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:10][C:11]2[CH:19]=[C:18]([C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[CH:17]=[C:16]3[C:12]=2[CH:13]=[N:14][NH:15]3)=[O:9])[C:5]([N:31]([CH3:32])[CH3:30])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 674DimethylamineHCID 81531DiisopropylethylamineHCID 44540868HCID 44540868、化合物

生成物 1

HCID 44539633HCID 44539633、化合物収率 201.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
160 °C

実験手順

6-Chloro-3-fluoro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-2-pyridinecarboxamide (188 mg, 0.46 mmol) was placed in a microwave vial and dissolved in THF (4 ml). Dimethylamine (0.463 ml, 0.93 mmol) and DIPEA (0.485 ml) were added and the mixture was heated at 160° C. for 1 h under microwave irradiation. The solvent was removed in vacuo and the yellow residue was dissolved in DCM (10 ml) and washed with water (10 ml). The DCM was removed in vacuo and the solid was dried in vacuo on a high vacuum line to afford the title compound (400 mg) as a yellow solid.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe yellow residue was dissolved in DCM (10 ml)
  3. washwashed with water (10 ml)
  4. customThe DCM was removed in vacuo
  5. customthe solid was dried in vacuo on a high vacuum line

出典と根拠

ORDレコード
ord-d746b15010074701a5bbe3ffd3df1833
出典データセット
uspto-grants-2014_07
特許番号
US08765743B2

反応ノート

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