Cesium carbonate → 5-Amino-7-(3,3-dimethyl-2-butanonyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

HRID 23136

반응식

HRID 23136 반응식
C([NH:8][N:9]1[C:15](=[O:16])[CH2:14][C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[C:11]2[CH:21]=[CH:22][CH:23]=[CH:24][C:10]1=2)(OC(C)(C)C)=O.C([O-])([O-])=O.[Cs+].[Cs+].[Cl:31][CH2:32][C:33](=[O:38])[C:34]([CH3:37])([CH3:36])[CH3:35]>CN(C=O)C.C(Cl)Cl>[ClH:31].[NH2:8][N:9]1[C:15](=[O:16])[CH:14]([CH2:32][C:33](=[O:38])[C:34]([CH3:37])([CH3:36])[CH3:35])[C:13]2[CH:12]=[CH:20][CH:19]=[CH:18][C:17]=2[C:24]2[CH:23]=[CH:22][CH:21]=[CH:11][C:10]1=2

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 835721-ChloropinacoloneHCID 114935485-(N-Boc-amino)-5,7-dihydro-6H-dibez[b,d]azepin-6-one

생성물 1

HCID 865851115-Amino-7-(3,3-dimethyl-2-butanonyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
60 °C

실험 절차

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (0.2 g, 0.617 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (0.3 g, 0.925 mmol) and warmed to 60° C. To the reaction mixture was added 1-chloro-3,3-dimethyl-2-butanone (0.096 ml, 0.74 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C., the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was isolated as a colorless solid.

후처리

  1. temperatureAfter cooling to 23° C.
  2. washwashed with several portions of brine
  3. dry with materialdried over Na2SO4

출처 및 근거

ORD 기록
ord-e296b3119fbd4a07a96185dcc917ec2c
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849650B2

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