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Sodium borohydride → Benzyl carbamate

HRID 38457
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HRID 38457 반응식
[CH2:1]([O:8][C:9](=[O:21])[NH:10]C1CC2C(=O)C(CSC2)C1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+]>C(O)C>[CH2:1]([O:8][C:9](=[O:21])[NH2:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydride3회HCID 67075315(9-Oxo-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester

생성물 1

HCID 12136Benzyl carbamate수율 40.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (9-oxo-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester (16, 4.2 g, 13.7 mmol) in ethanol (172 ml) was added sodium borohydride (0.78 g, 20.6 mmol) portionwise at room temperature. The solution was stirred for 1 hour before addition of sodium borohydride (0.2 g, 5 mmol). The reaction mixture was stirred for 2 days, a further portion of sodium borohydride (0.340 g, 9 mmol) was added, and stirring was continued for 4 hours. The mixture was then concentrated under reduced pressure and cold water was added to the residue as well as dichloromethane. After a extraction of the aqueous phase with dichlormethane, the combined organic layer was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (cyclohexane:ethyl acetate 40:60) to yield 9-hydroxy-3-thia-bicyclo[3.3.1]non-7-yl)-carbamic acid benzyl ester as a white solid (0.84 g).

후처리

  1. stirringstirring
  2. waitwas continued for 4 hours
  3. concentrationThe mixture was then concentrated under reduced pressure and cold water
  4. additionwas added to the residue as well as dichloromethane
  5. extractionAfter a extraction of the aqueous phase with dichlormethane
  6. dry with materialthe combined organic layer was dried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe crude product was purified by silica gel chromatography (cyclohexane:ethyl acetate 40:60)

출처 및 근거

ORD 기록
ord-70139663ca2642c695959b34bd86fff4
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524737B2

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