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

Methanol → 4-(5-Bromopyrimidin-2-yl)-3,5-difluorophenol

HRID 42007
ノート
印刷プレビュー

反応式

HRID 42007 の反応式
[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8]2[C:13]([F:14])=[CH:12][C:11]([O:15]C)=[CH:10][C:9]=2[F:17])=[N:6][CH:7]=1.B(Br)(Br)Br.CO.C([O-])(O)=O.[Na+]>C(Cl)Cl.C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[N:6][C:5]([C:8]2[C:9]([F:17])=[CH:10][C:11]([OH:15])=[CH:12][C:13]=2[F:14])=[N:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 673942495-Bromo-2-(2,6-difluoro-4-methoxyphenyl)pyrimidine

生成物 1

HCID 1361955854-(5-Bromopyrimidin-2-yl)-3,5-difluorophenol収率 96.5%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 5-bromo-2-(2,6-difluoro-4-methoxyphenyl)pyrimidine (0.887 g, 2.95 mmol) in DCM at 0° C., was added dropwise a solution of BBr3 (1M in DCM) (22 ml, 22 mmol) and the reaction mixture was stirred overnight at room temperature. This mixture was then poured over cold MeOH and solid NaHCO3 was added slowly until pH=4-5. The suspension obtained was filtered and the filtrate evaporated. The solid obtained was redissolved in ethyl acetate, washed with water and brine, dried and concentrated to give the desired compound as a white solid (0.817 g, 85% of yield).

後処理

  1. additionwas added slowly until pH=4-5
  2. customThe suspension obtained
  3. filtrationwas filtered
  4. customthe filtrate evaporated
  5. customThe solid obtained
  6. washwashed with water and brine
  7. customdried
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-18d6551235cd4ddda8d73eb9a4e6944b
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08536165B2

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