Water → 1-[4-(Hydroxymethyl)piperidin-1-yl]ethan-1-one

HRID 1199038ノート

反応式

HRID 1199038 の反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.[OH:8][CH2:9][N:10]1[CH2:15][CH2:14]C[CH2:12][CH2:11]1.O.[C:17](=O)([O-])[O-].[K+].[K+]>C(O)C>[C:9]([N:10]1[CH2:15][CH2:14][CH:6]([CH2:5][OH:7])[CH2:12][CH2:11]1)(=[O:8])[CH3:17]

参加物

6

反応物 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 446909Piperidin-1-ylmethanol

生成物 1

HCID 189349231-[4-(Hydroxymethyl)piperidin-1-yl]ethan-1-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
20 °C

実験手順

1-Acetyl-4-hydroxymethylpiperidine may be obtained in the following manner: acetic anhydride (20.5 cc) is added in the course of 15 minutes to a solution of hydroxymethylpiperidine (23.8 g) in ethanol (100 cc) at a temperature in the region of 10° C., and the mixture is stirred for 18 hours at a temperature in the region of 20° C. The reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa); the residue obtained is taken up with water (50 cc) and potassium carbonate (50 g), and the solution is extracted with methylene chloride (3×150 cc); the organic extracts are combined, dried and concentrated to dryness under reduced pressure (2.7 kPa). 1-Acetyl-4-hydroxymethylpiperidine (33.6 g) is thereby obtained in the form of an oil, which is employed in the crude state in the subsequent syntheses.

後処理

  1. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  2. customthe residue obtained
  3. extractionthe solution is extracted with methylene chloride (3×150 cc)
  4. customdried
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

出典と根拠

ORDレコード
ord-d7b77a4f19934657aad1f55d5fca907b
出典データセット
uspto-grants-1990_02
特許番号
US04898871

反応ノート

読み込み中…