Thioacetamide → (2-Methyl-4,5-dihydro-3-thia-1,6-diaza-benzo[e]azulen-6-yl)-phenyl-methanone

HRID 220786노트

반응식

HRID 220786 반응식
[C:1]([N:9]1[CH2:15][CH2:14][CH:13](Br)[C:12](=O)[C:11]2[CH:18]=[CH:19][CH:20]=[CH:21][C:10]1=2)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([NH2:25])(=[S:24])[CH3:23]>C(O)C>[CH3:23][C:22]1[S:24][C:13]2[CH2:14][CH2:15][N:9]([C:1]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)=[O:8])[C:10]3[CH:21]=[CH:20][CH:19]=[CH:18][C:11]=3[C:12]=2[N:25]=1

참가 물질

4

반응물 2

HCID 2723949ThioacetamideHCID 231123501-Benzoyl-4-bromo-1,2,3,4-tetrahydro-benzo[b]azepin-5-one

생성물 1

HCID 23112323(2-Methyl-4,5-dihydro-3-thia-1,6-diaza-benzo[e]azulen-6-yl)-phenyl-methanone수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 1-benzoyl-4-bromo-1,2,3,4-tetrahydrobenzo[b]azepin-5-one (11.0 g, 2.9 mmol) from Example E5.7 in ethanol (50 ml) was added thioacetamide (0.75 g, 10 mmol). The solution was stirred for 16 h. The resultant suspension was reduced in volume by evaporation and cooled. The precipitate was collected by filtration and the solid was washed with cold ethanol and dried to yield the title compound as a white solid (0.65 g, 70%).

후처리

  1. customThe resultant suspension was reduced in volume by evaporation
  2. temperaturecooled
  3. filtrationThe precipitate was collected by filtration
  4. washthe solid was washed with cold ethanol
  5. customdried

출처 및 근거

ORD 기록
ord-aabd500b712c4d4086ad85fec0c06704
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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