Sodium Bicarbonate → 1-Benzyl-3,3-difluoropiperidine-4,4-diol

HRID 451558노트

반응식

HRID 451558 반응식
[CH2:1]([N:8]1[CH2:13][C:12]([F:15])([F:14])[C:11](=[O:16])[CH:10](C(OCC)=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(O)=[O:23].[Na+]>Cl>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11]([OH:16])([OH:23])[C:12]([F:14])([F:15])[CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 49761228Ethyl 1-benzyl-5,5-difluoro-4-oxopiperidine-3-carboxylate

생성물 1

HCID 574158661-Benzyl-3,3-difluoropiperidine-4,4-diol

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of ethyl 1-benzyl-5,5-difluoro-4-oxopiperidine-3-carboxylate (4.272 g, 14.4 mmol) dissolved in 3 N HCl (175 mL) was heated at reflux for 14 hours. The reaction mixture was cooled to room temperature, then solid NaHCO3 was added until pH 8 and extracted three times with ethyl acetate, the combined organic layers were dried over Na2SO4 and the solvents were evaporated. The title compound was obtained as white solid (3.5 g, 100%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 14 hours
  3. extractionextracted three times with ethyl acetate
  4. dry with materialthe combined organic layers were dried over Na2SO4
  5. customthe solvents were evaporated

출처 및 근거

ORD 기록
ord-dab1da1d31fb4a0ca2b2f2cda9c71ec4
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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