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Water → Benzyl [4-(3-hydroxy-1-methylpiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate

HRID 518807
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HRID 518807 반응식
[BH4-].[Na+].[CH3:3][N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[C:12]([O:27][CH:28]([CH3:30])[CH3:29])[CH:11]=2)[C:6](=[O:31])[CH2:5]1.O.[Cl-].[Na+]>C(O)C.C(OCC)(=O)C>[OH:31][CH:6]1[CH:7]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:26])[O:18][CH2:19][C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)=[C:12]([O:27][CH:28]([CH3:29])[CH3:30])[CH:11]=2)[CH2:8][CH2:9][N:4]([CH3:3])[CH2:5]1
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참가 물질

7

반응물 4

HCID 962WaterHCID 5234Sodium ChlorideHCID 4311764Sodium borohydrideHCID 86697978Benzyl [4-(1-methyl-3-oxopiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate

생성물 1

HCID 86697979Benzyl [4-(3-hydroxy-1-methylpiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate수율 26%

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 8857Ethyl Acetate용매

실험 절차

486 mg of NaBH4 are added, in portions, to a suspension of 700 mg of benzyl [4-(1-methyl-3-oxopiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate in 35 ml of ethanol brought to 5° C. The reaction medium is stirred at ambient temperature for 50 minutes. 4 ml of water, 15 ml of a saturated aqueous sodium chloride solution and 40 ml of ethyl acetate are added. The two phases are separated, and the aqueous phase is washed with twice 20 ml of ethyl acetate. The combined organic phases are dried over magnesium sulfate, filtered and evaporated. Purification is carried out by flash chromatography on silica gel (40-63 μm), elution being carried out with a mixture of dichloromethane and (MeOH+10% NH4OH) (99/1 to 90/10). 183 mg of benzyl [4-(3-hydroxy-1-methylpiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate (trans diastereoisomers) and 183 mg of benzyl [4-(3-hydroxy-1-methylpiperidin-4-yl)-2-(propan-2-yloxy)phenyl]carbamate (cis diastereoisomers) are obtained.

후처리

  1. custombrought to 5° C
  2. customThe two phases are separated
  3. washthe aqueous phase is washed with twice 20 ml of ethyl acetate
  4. dry with materialThe combined organic phases are dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customPurification
  8. washis carried out by flash chromatography on silica gel (40-63 μm), elution
  9. additionbeing carried out with a mixture of dichloromethane and (MeOH+10% NH4OH) (99/1 to 90/10)

출처 및 근거

ORD 기록
ord-fb9b42a93e94437c9ac4aa2a8d3da8a8
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115140B2

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