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

HRID 451558ノート

反応式

HRID 451558 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-dab1da1d31fb4a0ca2b2f2cda9c71ec4
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

反応ノート

読み込み中…