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

HRID 980168ノート

反応式

HRID 980168 の反応式
[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

参加物

5

反応物 2

HCID 6259Phenacyl bromideHCID 119590965-Iodopyrimidin-2-ol

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e03a08e39a184094a14204bdf2a65dc9
出典データセット
uspto-grants-1987_01
特許番号
US04636509

反応ノート

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