Water → 5-Chloro-1-(2-oxo-2-phenylethyl)-2(1H)-pyrimidinone

HRID 980189노트

반응식

HRID 980189 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:17])[N:6]([CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2O)[CH:7]=1.[OH2:18]>N1C=CC=CC=1.[O-2].[O-2].[O-2].[Cr+6]>[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:17])[N:6]([CH2:8][C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:18])[CH:7]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 20222325HCID 20222325, 화합물

생성물 1

HCID 127955325-Chloro-1-(2-oxo-2-phenylethyl)-2(1H)-pyrimidinone

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 1049Pyridine용매2회

실험 절차

A solution of 5-chloro-1-(2-hydroxyphenethyl)pyrimidin-2-one (251 mg) in pyridine (6 ml) was added to the stirred suspension obtained by adding chromium trioxide (408 mg) to pyridine (4 ml). After 21/2 hours the mixture was diluted with water (10 ml) and the products were extracted with ethyl acetate (150 ml). The extract was washed with N-hydrochloric acid (2×25 ml) and water (50 ml), dried (MgSO4) and evaporated to a solid (271 mg). Crystallisation of this from ethanol followed by purification of the mother liquor material by preparative-layer chromatography gave the title pyrimidinone (48 mg), whose p.m.r. spectrum (in deuteriodimethylsulphoxide) and t.l.c. characteristics were identical to those of authentic material (vide supra).

후처리

  1. customobtained
  2. extractionthe products were extracted with ethyl acetate (150 ml)
  3. washThe extract was washed with N-hydrochloric acid (2×25 ml) and water (50 ml)
  4. dry with materialdried (MgSO4)
  5. customevaporated to a solid (271 mg)
  6. customCrystallisation of this from ethanol
  7. customfollowed by purification of the mother liquor material by preparative-layer chromatography

출처 및 근거

ORD 기록
ord-84afefc56f0244d2a5927d2dc6be50de
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636509

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