Cesium carbonate → HCID 178498214, 화합물

HRID 2235239노트

반응식

HRID 2235239 반응식
[C:1]([Si:5]([CH3:30])([CH3:29])[O:6][C@@H:7]1[CH2:12][CH2:11][C@H:10]([N:13]2[CH2:17][CH2:16][CH:15]([CH2:18][C:19]3[C:24]([Cl:25])=[CH:23][C:22]([OH:26])=[CH:21][C:20]=3[Cl:27])[C:14]2=[O:28])[CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].[C:31]([O-])([O-])=O.[Cs+].[Cs+].FC[C:39]1[CH:47]=[CH:46][C:42]([C:43]([O-:45])=[O:44])=[CH:41][CH:40]=1>CN(C=O)C.O.CCOC(C)=O>[CH3:31][O:45][C:43](=[O:44])[C:42]1[CH:46]=[CH:47][C:39]([O:26][C:22]2[CH:21]=[C:20]([Cl:27])[C:19]([CH2:18][CH:15]3[CH2:16][CH2:17][N:13]([C@H:10]4[CH2:11][CH2:12][C@@H:7]([O:6][Si:5]([C:1]([CH3:2])([CH3:4])[CH3:3])([CH3:30])[CH3:29])[CH2:8][CH2:9]4)[C:14]3=[O:28])=[C:24]([Cl:25])[CH:23]=2)=[CH:40][CH:41]=1

참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 17850960p-FluoromethylbenzoateHCID 178455342HCID 178455342, 화합물

생성물 1

HCID 178498214HCID 178498214, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Combine 0.5 g (1 mmol) of 1-[cis-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-3-(2,6-dichloro-4-hydroxy-benzyl)-pyrrolidin-2-one (Preparation 72) 0.7 g (2 mmol) Cs2CO3 and 0.49 g (3 mmol) p-fluoromethylbenzoate in 10 mL dry DMF and heat at 100° C. for 4 hours. Dilute the mixture with 25 mL H2O and 50 mL EtOAc. Separate the layers and extract the aqueous with 50 mL EtOAc. Combine the organic layers, wash with brine, dry over MgSO4 and concentrate under vacuum. Purify via chromatography using 30% EtOAc in hexanes to recover 0.47 g of an oil.

후처리

  1. customSeparate the layers
  2. extractionextract the aqueous with 50 mL EtOAc
  3. washwash with brine
  4. dry with materialdry over MgSO4
  5. concentrationconcentrate under vacuum
  6. customPurify via chromatography
  7. customto recover 0.47 g of an oil

출처 및 근거

ORD 기록
ord-64eb0807e57c4d5eb17d86359732c21f
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713979B2

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