Acetic Acid → tert-Butyl (1-isopropylpiperidin-4-yl)carbamate

HRID 18505

반응식

HRID 18505 반응식
[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[C:15](O)(=O)[CH3:16].[CH3:19]O>CC(C)=O>[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([CH:15]([CH3:16])[CH3:19])[CH2:10][CH2:9]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 887MethanolHCID 7238334-(N-Boc-amino)piperidine

생성물 1

HCID 20801240tert-Butyl (1-isopropylpiperidin-4-yl)carbamate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 5.0 g Piperidin-4-yl-carbamic acid tert-butyl ester in 15 mL methanol, 7.34 mL acetone, 3.14 g Na(CN)BH3 and 0.3 mL acetic acid were added. After stirring for 16 h at room temperature the solvent was removed under reduced pressure and the residue was partitioned between 30 mL water and 30 mL ethyl acetate. The organic layer was washed with saturated Na2CO3 solution, water and then dried over Na2SO4. The solvent was removed under reduced pressure to give the product as a white solid. Yield: 4.8 g MS (ES+): m/e=243.

후처리

  1. customwas removed under reduced pressure
  2. customthe residue was partitioned between 30 mL water and 30 mL ethyl acetate
  3. washThe organic layer was washed with saturated Na2CO3 solution, water
  4. dry with materialdried over Na2SO4
  5. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-68c78e6687d943f586a73639b91bb8f8
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741341B2

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