ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Bromine → 5-Bromo-3-methyl-6-phenyl-4-pyrimidinone

HRID 1981587
ノート
印刷プレビュー

反応式

HRID 1981587 の反応式
N[C:2]1[N:7]([CH3:8])[C:6](=[O:9])[CH:5]=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:3]=1.[Br:16]Br>CC(O)=O>[Br:16][C:5]1[C:6](=[O:9])[N:7]([CH3:8])[CH:2]=[N:3][C:4]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24408BromineHCID 133205052-Amino-3-methyl-6-phenyl-4-pyrimidinone

生成物 1

HCID 233196395-Bromo-3-methyl-6-phenyl-4-pyrimidinone収率 42.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To 1.8 g (8.95 mM) of 2-amino-3-N-methyl-6-phenyl-4-pyrimidinone was added 40 ml CH3COOH and 0.535 ml Br2 (1.64 g≈10.3 mM). The reaction mixture was allowed to stir at ambient temperature for 18 hours. The solution was evaporated to dryness and the residual solid azeotroped from EtOH (2X). The solids were heated to reflux with 100 ml of H2O, cooled to 5° and filtered. This procedure was repeated, filtered hot, and allowed to crystallize at room temperature for 18 hours. The crystals were filtered and washed well with H2O to yield 1.0 g (40%) of title compound. Cooling of mother liquors gave an additional 0.6 g (24%) of title compound.

後処理

  1. customThe solution was evaporated to dryness
  2. customthe residual solid azeotroped from EtOH (2X)
  3. temperatureThe solids were heated
  4. temperatureto reflux with 100 ml of H2O
  5. temperaturecooled to 5°
  6. filtrationfiltered
  7. filtrationfiltered hot
  8. customto crystallize at room temperature for 18 hours
  9. filtrationThe crystals were filtered
  10. washwashed well with H2O

出典と根拠

ORDレコード
ord-30bd46901dff47dd969fadecbb88551e
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04593096

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート