Cesium carbonate → HCID 178498214、化合物

HRID 2235239ノート

反応式

HRID 2235239 の反応式
[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

参加物

7

反応物 3

HCID 10796Cesium carbonateHCID 17850960p-FluoromethylbenzoateHCID 178455342HCID 178455342、化合物

生成物 1

HCID 178498214HCID 178498214、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-64eb0807e57c4d5eb17d86359732c21f
出典データセット
uspto-grants-2010_05
特許番号
US07713979B2

反応ノート

読み込み中…