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Potassium Carbonate → HCID 178432322, 화합물

HRID 220781
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HRID 220781 반응식
[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
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참가 물질

6

반응물 3

HCID 11430Potassium Carbonate3회HCID 67170Acetamidine monohydrochloride3회HCID 231123501-Benzoyl-4-bromo-1,2,3,4-tetrahydro-benzo[b]azepin-5-one

생성물 2

HCID 231123696-benzoyl-2-methyl-5,6-dihydro-4H-1-oxa-3,6-diaza-benzo[e]azulene수율 4%HCID 178432322HCID 178432322, 화합물수율 34%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-40ee044daf72473a993137e1df243929
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202858B2

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