Hydrochloric Acid → 1-Benzoylpiperidine-4-carboxylic acid

HRID 617192

反応式

HRID 617192 の反応式
[NH:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[C:16](Cl)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl>O>[C:16]([N:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 37734-Piperidinecarboxylic acidHCID 7412Benzoyl chlorideHCID 11430Potassium Carbonate

生成物 1

HCID 789351-Benzoylpiperidine-4-carboxylic acid収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To an ice cold solution of isonipecotic acid (90 g, 0.697 mol) and potassium carbonate (81 g, 1.31 mol) in water (1.3 liter) was added dropwise benzoyl chloride (81 ml, 0.697 mol) over a period of about an hour at about 5° C. The mixture was stirred at room temperature overnight. The reaction mixture was acidified with 6N hydrochloric acid and extracted with dichloromethane. The organic layer was washed with water and then dried over magnesium sulfate and the solvent was evaporated in vacuo. Crystallization from isopropyl alcohol-diethyl ether to give the titled compound (154.4 g).

後処理

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was evaporated in vacuo
  5. customCrystallization from isopropyl alcohol-diethyl ether

出典と根拠

ORDレコード
ord-090031d131f24188b7adc55f41b6ba9b
出典データセット
uspto-grants-1999_09
特許番号
US05948786

関連ノート

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