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

HRID 1678248노트

반응식

HRID 1678248 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 554404Methyl chloromethanethioateHCID 59023728HCID 59023728, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e270663c97304f4bb9384348b20cbc6c
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08008481B2

반응 노트

불러오는 중…