Cesium carbonate → HCID 71144315, 화합물

HRID 509363노트

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HRID 509363 반응식
[F:1][C:2]1[C:3]([C@H:8]([C:19]2[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:27])[F:26])=[CH:21][CH:20]=2)[NH:9][C:10](=[O:18])[C:11]2[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][N:12]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.C([O:33][C:34](=[O:37])[CH2:35]Br)(C)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+]>C(Cl)Cl.CN(C=O)C>[F:1][C:2]1[C:3]([C@@H:8]([NH:9][C:10]([C:11]2[N:12]=[CH:13][C:14]([O:17][CH2:35][C:34]([OH:37])=[O:33])=[CH:15][CH:16]=2)=[O:18])[C:19]2[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:26])[F:27])=[CH:21][CH:20]=2)=[N:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 79177tert-Butyl bromoacetateHCID 71144553HCID 71144553, 화합물

생성물 1

HCID 71144315HCID 71144315, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of (S)—N-((3-fluoropyridin-2-yl)(4-(trifluoromethyl)phenyl)-methyl)-5-hydroxypicolinamide (Example 173) (0.145 g, 0.371 mmol) in DCM (2 mL) and DMF (0.2 mL) were added bromoacetic acid t-butyl ester (0.072 mL, 0.445 mmol) and cesium carbonate (0.241 g, 0.741 mmol). The resulting mixture was then stirred at rt for 2 h. Then, the mixture was filtered and the solid was washed with DCM (1×1 mL) and MeOH (1×1 mL). The combined filtrates were concentrated and dried to give the desired product, which was used without further purification in the next step.

후처리

  1. filtrationThen, the mixture was filtered
  2. washthe solid was washed with DCM (1×1 mL) and MeOH (1×1 mL)
  3. concentrationThe combined filtrates were concentrated
  4. customdried

출처 및 근거

ORD 기록
ord-6da639b223b4495690c9902de93d0a88
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096527B2

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