Triethylamine → (7-benzo[b]thiophen-2-yl-1H-indazol-5-yl)-thiocarbamic acid S-methyl ester

HRID 1678248ノート

反応式

HRID 1678248 の反応式
[S:1]1[C:5]([C:6]2[CH:7]=[C:8]([NH2:15])[CH:9]=[C:10]3[C:14]=2[NH:13][N:12]=[CH:11]3)=[CH:4][C:3]2[CH:16]=[CH:17][CH:18]=[CH:19][C:2]1=2.Cl[C:21]([O:23]C)=[S:22].[CH2:25](N(CC)CC)C>C(O)C>[CH3:25][S:23][C:21](=[O:22])[NH:15][C:8]1[CH:9]=[C:10]2[C:14](=[C:6]([C:5]3[S:1][C:2]4[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=4[CH:4]=3)[CH:7]=1)[NH:13][N:12]=[CH:11]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 554404Methyl chloromethanethioateHCID 59023728HCID 59023728、化合物

生成物 1

HCID 59023854(7-benzo[b]thiophen-2-yl-1H-indazol-5-yl)-thiocarbamic acid S-methyl ester収率 66%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 7-benzo[b]thiophen-2-yl-1H-indazol-5-ylamine (Example #F.8.1, 530 mg, 2.0 mmol) and methyl chlorothioformate (0.25 mL, 2.8 mmol) in ethanol (10 mL) was added triethylamine (0.56 mL, 4.0 mmol). The reaction mixture was stirred at ambient temperature for about 16 hours and the resulting solid was collected by filtration, washed with water (3×50 mL), and dried to yield (7-benzo[b]thiophen-2-yl-1H-indazol-5-yl)-thiocarbamic acid S-methyl ester (448 mg, 66%); LC/MS (Table 1, Method e) Rt 2.14 min; m/z: [M−H]− 338.

後処理

  1. filtrationthe resulting solid was collected by filtration
  2. washwashed with water (3×50 mL)
  3. customdried

出典と根拠

ORDレコード
ord-e270663c97304f4bb9384348b20cbc6c
出典データセット
uspto-grants-2011_08
特許番号
US08008481B2

反応ノート

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