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

HRID 220786ノート

反応式

HRID 220786 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-aabd500b712c4d4086ad85fec0c06704
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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