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

HRID 1199038노트

반응식

HRID 1199038 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d7b77a4f19934657aad1f55d5fca907b
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898871

반응 노트

불러오는 중…