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Potassium Carbonate → HCID 178432322、化合物

HRID 220781
ノート
印刷プレビュー

反応式

HRID 220781 の反応式
[C:1]([N:9]1[CH2:15][CH2:14][CH:13](Br)[C:12](=[O:17])[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.Cl.[C:23]([NH2:26])(=[NH:25])[CH3:24].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:1]([N:9]1[CH2:15][CH2:14][C:13]2[N:26]=[C:23]([CH3:24])[NH:25][C:12]=2[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:1]([N:9]1[CH2:15][CH2:14][C:13]2[N:25]=[C:23]([CH3:24])[O:17][C:12]=2[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium Carbonate3 回HCID 67170Acetamidine monohydrochloride3 回HCID 231123501-Benzoyl-4-bromo-1,2,3,4-tetrahydro-benzo[b]azepin-5-one

生成物 2

HCID 231123696-benzoyl-2-methyl-5,6-dihydro-4H-1-oxa-3,6-diaza-benzo[e]azulene収率 4%HCID 178432322HCID 178432322、化合物収率 34%

試薬・触媒・溶媒

1
HCID 6342Acetonitrile溶媒

実験手順

1-Benzoyl-4-bromo-1,2,3,4-tetrahydro-benzo[b]azepin-5-one (67.5 g, 200 mmol) from Example E5.7, acetamidine hydrochloride (92.7 g, 980 mmol) and potassium carbonate (136.0 g, 980 mmol) were suspended in acetonitrile (2.0 liters) and heated at reflux for 17 h under nitrogen. Additional acetamidine hydrochloride (18.5 g, 200 mmol) and potassium carbonate (27.7 g, 200 mmol) were added and the reaction mixture was heated at reflux for a further 6 h. Additional acetamidine hydrochloride (18.5 g, 200 mmol) and potassium carbonate (27.7 g, 200 mmol) were added again and the reaction mixture was heated at reflux for a further 6 h. On cooling to room temperature, the reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was taken up in dichloromethane (1.4 liters), washed with water (500 ml), dried over sodium sulfate, filtered and reduced in vacuo. The crude products were purified by flash chromatography on silica gel (eluant; 45% EtOAc:45% acetonitrile: 10% methanol) to yield the title compound (26.7 g, 34%) and 6-benzoyl-2-methyl-5,6-dihydro-4H-1-oxa-3,6-diaza-benzo[e]azulene (3.3 g, 4%).

後処理

  1. temperatureheated
  2. temperatureat reflux for 17 h under nitrogen
  3. temperaturethe reaction mixture was heated
  4. temperatureat reflux for a further 6 h
  5. temperaturethe reaction mixture was heated
  6. temperatureat reflux for a further 6 h
  7. filtrationthe reaction mixture was filtered
  8. concentrationthe filtrate was concentrated in vacuo
  9. washwashed with water (500 ml)
  10. dry with materialdried over sodium sulfate
  11. filtrationfiltered
  12. customThe crude products were purified by flash chromatography on silica gel (eluant; 45% EtOAc:45% acetonitrile: 10% methanol)

出典と根拠

ORDレコード
ord-40ee044daf72473a993137e1df243929
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202858B2

反応ノート

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