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

HRID 459996ノート

反応式

HRID 459996 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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 of 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: 4.8g. MS (ES+): m/e=243.

後処理

  1. customwas removed under reduced pressure
  2. customthe residue was partitioned between 30 ml of 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

出典と根拠

ORDレコード
ord-3d83b21497d040eab23e67c48dd37798
出典データセット
uspto-grants-2007_03
特許番号
US07196103B2

反応ノート

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