ethyl 5-{[(1-methyl-1-phenylethyl)amino]carbonyl}-3-[(4-morpholin-4-ylbenzoyl)amino]-1H-thieno[2,3-c]pyrazole-1-carboxylate → HCID 178457636、化合物

HRID 1096158ノート

反応式

HRID 1096158 の反応式
[CH3:1][C:2]([NH:10][C:11]([C:13]1[S:40][C:16]2[N:17](C(OCC)=O)[N:18]=[C:19]([NH:20][C:21](=[O:34])[C:22]3[CH:27]=[CH:26][C:25]([N:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[CH:24][CH:23]=3)[C:15]=2[CH:14]=1)=[O:12])([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH3:3]>CO.C(N(CC)CC)C>[CH3:3][C:2]([NH:10][C:11]([C:13]1[S:40][C:16]2[NH:17][N:18]=[C:19]([NH:20][C:21](=[O:34])[C:22]3[CH:27]=[CH:26][C:25]([N:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[CH:24][CH:23]=3)[C:15]=2[CH:14]=1)=[O:12])([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1)[CH3:1]

参加物

4

反応物 1

HCID 44520544ethyl 5-{[(1-methyl-1-phenylethyl)amino]carbonyl}-3-[(4-morpholin-4-ylbenzoyl)amino]-1H-thieno[2,3-c]pyrazole-1-carboxylate

生成物 1

HCID 178457636HCID 178457636、化合物収率 86.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8471Triethylamine溶媒

反応条件

温度
70 °C

実験手順

A suspension of ethyl 5-{[(1-methyl-1-phenylethyl)amino]carbonyl}-3-[(4-morpholin-4-ylbenzoyl)amino]-1H-thieno[2,3-c]pyrazole-1-carboxylate (3.71 g, 6.6 mmol) in methanol (MeOH, 70 mL) and triethylamine (TEA, 7 mL) was stirred at 70° C. for 5 hours. After evaporation of the solvent under reduced pressure, the residue was taken up with DCM and washed with water. The organic layer was separated, dried over sodium sulfate and evaporated. Purification by chromatography (DCM/MeOH 47:3) gave 2.8 g of the title compound.

後処理

  1. customAfter evaporation of the solvent under reduced pressure
  2. washwashed with water
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customPurification by chromatography (DCM/MeOH 47:3)

出典と根拠

ORDレコード
ord-7fcf0f38faa048b7aef681ca041ff388
出典データセット
uspto-grants-2012_03
特許番号
US08138217B2

反応ノート

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