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

HRID 980189ノート

反応式

HRID 980189 の反応式
[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

参加物

5

反応物 2

HCID 962WaterHCID 20222325HCID 20222325、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 10219390chromium (VI) trioxide触媒HCID 1049Pyridine溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-84afefc56f0244d2a5927d2dc6be50de
出典データセット
uspto-grants-1987_01
特許番号
US04636509

反応ノート

読み込み中…