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Water → (3S,4S)-4-(1-(R)-carboxyethyl)-3-(1-(R)-benzyloxycarbonyloxyethyl)-2-azetidinone

HRID 21720
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HRID 21720 반응식
[OH:1][CH2:2][C@@H:3]([C@@H:5]1[NH:8][C:7](=[O:9])[C@@H:6]1[C@H:10]([O:12][C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14])[CH3:11])[CH3:4].CC(C)=[O:25].OS(O)(=O)=O.O=[Cr](=O)=O.S(=O)(=O)(O)O.O>CC(C)=O.[O-2].[O-2].[O-2].[Cr+6]>[C:2]([C@@H:3]([C@H:5]1[NH:8][C:7](=[O:9])[C@@H:6]1[C@H:10]([O:12][C:13]([O:15][CH2:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)=[O:14])[CH3:11])[CH3:4])([OH:25])=[O:1]
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HCID 962WaterHCID 1118Sulfuric AcidHCID 13960427(3S,4S)-4-(1-(R)-hydroxymethylethyl)-3-(1-(R)-benzyloxycarbonyloxyethyl)-2-azetidinoneHCID 131709961Jones' reagent

생성물 1

HCID 13960430(3S,4S)-4-(1-(R)-carboxyethyl)-3-(1-(R)-benzyloxycarbonyloxyethyl)-2-azetidinone

시약·촉매·용매 2

HCID 10219390
chromium (VI) trioxide
촉매
HCID 180Acetone용매

실험 절차

A solution of (3S,4S)-4-(1-(R)-hydroxymethylethyl)-3-(1-(R)-benzyloxycarbonyloxyethyl)-2-azetidinone (6.1 g) in acetone (60 ml) was treated with the Jones reagent, prepared from chromium trioxide (2.78 g), 98% sulfuric acid (4.4 g) and water (8.1 ml), at 10°-20° C. for 1 hour. The reaction mixture was quenched with isopropanol (0.5 ml) at 10°-20° C. for 15 minutes, diluted with ethyl acetate (122 ml) and washed with water (135 ml). The aqueous layer was separated from the organic layer and extracted with ethyl acetate (61 ml). The ethyl acetate extracts and the organic layer were combined together and extracted with 5% aqueous sodium bicarbonate solution (30 ml). The extract was washed with dichloromethane (60 ml) and acidified with 10% hydrochloric acid solution (20 ml) with ice-cooling. The acidic solution was extracted twice with dichloromethane (60 ml). The extracts were washed with brine and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated in vacuo to give (3S,4S)-4-(1-(R)-carboxyethyl)-3-(1-(R)-benzyloxycarbonyloxyethyl)-2-azetidinone.

후처리

  1. customThe reaction mixture was quenched with isopropanol (0.5 ml) at 10°-20° C. for 15 minutes
  2. additiondiluted with ethyl acetate (122 ml)
  3. washwashed with water (135 ml)
  4. customThe aqueous layer was separated from the organic layer
  5. extractionextracted with ethyl acetate (61 ml)
  6. extractionextracted with 5% aqueous sodium bicarbonate solution (30 ml)
  7. washThe extract was washed with dichloromethane (60 ml)
  8. temperaturecooling
  9. extractionThe acidic solution was extracted twice with dichloromethane (60 ml)
  10. washThe extracts were washed with brine
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationAfter filtration
  13. concentrationthe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-b76297b7782a4dedb693a126d3a0daab
출처 데이터셋
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05424422

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