Phenacyl bromide → 5-Iodo-1-phenacylpyrimidin-2-one

HRID 980168노트

반응식

HRID 980168 반응식
[I:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.Br[CH2:10][C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:12]>C(N(CC)CC)C.C(O)C>[I:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[N:6]([CH2:10][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:12])[CH:7]=1

참가 물질

5

반응물 2

HCID 6259Phenacyl bromideHCID 119590965-Iodopyrimidin-2-ol

생성물 1

HCID 127955355-Iodo-1-phenacylpyrimidin-2-one

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

실험 절차

A suspension of 5-iodopyrimidin-2-one (556 mg) and α-bromoacetophenone (533 mg) in triethylamine (0.5 ml) and ethanol (50 ml) was stirred at ambient temperature for 71/2 hours. The resulting solution was evaporated and the residue triturated with water. This product was purified by preparative thin-layer chromatography on silica before crystallisation from ethyl acetate to give the title pyrimidinone: yield 253 mg: m.p. 155°-157°: λmaxEtOH 238.5 nm (ε 23070), 340 nm (ε 2400), λinf 250 nm (ε 17160), 275 nm (ε 1780).

후처리

  1. customThe resulting solution was evaporated
  2. customthe residue triturated with water
  3. customThis product was purified by preparative thin-layer chromatography on silica before crystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-e03a08e39a184094a14204bdf2a65dc9
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636509

반응 노트

불러오는 중…