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Acetone → tert-butyl (6R,7R)-6-(3,4-dichlorophenyl)-7-[(1S)-1,2-dihydroxyethyl]-1,4-oxazepane-4-carboxylate

HRID 1022649
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HRID 1022649 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H](C=C)O[CH2:13][CH2:12][N:11]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].C[N+]1([O-])CC[O:29]CC1.[CH3:33][C:34]([CH3:36])=[O:35].[OH2:37]>C(#N)C.[Os](=O)(=O)(=O)=O>[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:33]([C@@H:34]([OH:35])[CH2:36][OH:29])[O:37][CH2:13][CH2:12][N:11]([C:18]([O:20][C:21]([CH3:22])([CH3:24])[CH3:23])=[O:19])[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 180AcetoneHCID 962WaterHCID 82029Methyl morpholine oxideHCID 66974991tert-butyl (6R,7S)-6-(3,4-dichlorophenyl)-7-ethenyl-1,4-oxazepane-4-carboxylate

생성물 1

HCID 66975748tert-butyl (6R,7R)-6-(3,4-dichlorophenyl)-7-[(1S)-1,2-dihydroxyethyl]-1,4-oxazepane-4-carboxylate

시약·촉매·용매 2

HCID 30318
Osmium Tetroxide
촉매
HCID 6342Acetonitrile용매

실험 절차

To a mixed solution of tert-butyl (6R,7S)-6-(3,4-dichlorophenyl)-7-ethenyl-1,4-oxazepane-4-carboxylate (1.08 g) and 4-methylmorpholine N-oxide (680 mg) in acetonitrile (6 mL)/acetone (6 mL)/water (6 ml) was added osmium(VIII) oxide immobilized catalyst I (Wako Pure Chemical Industries, Ltd. cat. 153-02581) (700 mg), and the mixture was stirred under nitrogen purging at room temperature overnight. The catalyst was filtered off through celite, and the filtrate was concentrated. Water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated (product about 1.07 g). 900 mg therefrom was purified by HPLC (column: Sunrise C18-SAC 20×150 mm, mobile phase: water/acetonitrile (containing 5 mM ammonium acetate)) to give the title compound (diastereomer having a shorter retention time) (610 mg) as a colorless oil.

후처리

  1. filtrationThe catalyst was filtered off through celite
  2. concentrationthe filtrate was concentrated
  3. additionWater was added
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated (product about 1.07 g)
  8. custom900 mg therefrom was purified by HPLC (column: Sunrise C18-SAC 20×150 mm, mobile phase: water/acetonitrile (containing 5 mM ammonium acetate))

출처 및 근거

ORD 기록
ord-c064bb15e4534bb08e9f555360fd9f4d
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

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