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Water → 2-Methyl-1-(4-methylamino-piperidin-1-yl)-propan-2-ol

HRID 1928879
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인쇄 미리보기

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HRID 1928879 반응식
C(O[C:4](=O)[NH:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][C:13]([OH:16])([CH3:15])[CH3:14])[CH2:8][CH2:7]1)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH3:15][C:13]([OH:16])([CH3:14])[CH2:12][N:9]1[CH2:10][CH2:11][CH:6]([NH:5][CH3:4])[CH2:7][CH2:8]1
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참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 68631449[1-(2-Hydroxy-2-methyl-propyl)-piperidin-4-yl]-carbamic acid ethyl ester

생성물 1

HCID 608856842-Methyl-1-(4-methylamino-piperidin-1-yl)-propan-2-ol수율 100%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

A mixture of the above described [1-(2-hydroxy-2-methyl-propyl)-piperidin-4-yl]-carbamic acid ethyl ester (2.35 g, 10 mmol) in tetrahydrofuran (40 mL) with lithium aluminum hydride (913 mg, 24 mmol) was refluxed for 16 h. Cooled to 0° C., added water (0.913 mL), then at 23° C. 15% NaOH solution (2.739 mL), then again water (0.913 mL), stirred at 23° C. for 30 min, filtered the solid off, washed with tetrahydrofuran, the filtrate was evaporated to give the title compound as a colorless oil (1.80 g, 100%); MS: m/e=187.2 (M+H+).

후처리

  1. additionA mixture of the
  2. temperaturewas refluxed for 16 h
  3. customat 23° C
  4. filtrationfiltered the solid off,
  5. washwashed with tetrahydrofuran
  6. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-a23d978cc4b34d8281c01b52fcf18319
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183380B2

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