Potassium → methyl 2-((3S)-6-((1R)-4-(2,6-dimethyl-4-(2-(methylsulfinyl)ethoxy)phenyl)-7-fluoro-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate

HRID 237449노트

반응식

HRID 237449 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][S:11][CH3:12])[CH:5]=[C:4]([CH3:13])[C:3]=1[C:14]1[CH:22]=[CH:21][C:20]([F:23])=[C:19]2[C:15]=1[CH2:16][CH2:17][C@H:18]2[O:24][C:25]1[CH:38]=[CH:37][C:28]2[C@H:29]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[CH2:30][O:31][C:27]=2[CH:26]=1.[K].[OH:40]OS([O-])=O.[K+]>CO.O>[CH3:13][C:4]1[CH:5]=[C:6]([O:8][CH2:9][CH2:10][S:11]([CH3:12])=[O:40])[CH:7]=[C:2]([CH3:1])[C:3]=1[C:14]1[CH:22]=[CH:21][C:20]([F:23])=[C:19]2[C:15]=1[CH2:16][CH2:17][C@H:18]2[O:24][C:25]1[CH:38]=[CH:37][C:28]2[C@H:29]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[CH2:30][O:31][C:27]=2[CH:26]=1

참가 물질

6

반응물 3

HCID 5462222PotassiumHCID 23707502Potassium hydroxy sulfiteHCID 86697114Methyl 2-((S)-6-((R)-4-(2,6-dimethyl-4-(2-(methylthio)ethoxy)phenyl)-7-fluoro-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate

생성물 1

HCID 86697370methyl 2-((3S)-6-((1R)-4-(2,6-dimethyl-4-(2-(methylsulfinyl)ethoxy)phenyl)-7-fluoro-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of methyl 2-((S)-6-((R)-4-(2,6-dimethyl-4-(2-(methylthio)ethoxy)phenyl)-7-fluoro-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate (230 mg) in methanol (4 mL) and water (2 mL) is added potassium peroxomonoslufate (Oxone®) (490 mg). The mixture is stirred for 1 hour at room temperature and then partitioned between dichloromethane and water. The organic phase is dried (MgSO4) and concentrated to give the crude product, which is directly in the next step. Yield: 220 mg; LC (method 4): tR=1.79 min; Mass spectrum (ESI+): m/z=553 [M+H]+.

후처리

  1. custompartitioned between dichloromethane and water
  2. dry with materialThe organic phase is dried (MgSO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2614800c9ef445559924f6e311ba48d9
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642585B2

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