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

Ammonia → 5-Bromo-2-(trifluoromethyl)pyrimidine

HRID 734336
ノート
印刷プレビュー

反応式

HRID 734336 の反応式
[F-].[K+].[F:3][C:4]([Si](C)(C)C)([F:6])[F:5].[Br:11][C:12]1[CH:13]=[N:14][C:15](I)=[N:16][CH:17]=1.N>CN1C(=O)CCC1.CN(C)C=O>[Br:11][C:12]1[CH:13]=[N:14][C:15]([C:4]([F:6])([F:5])[F:3])=[N:16][CH:17]=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 222AmmoniaHCID 522689Potassium FluorideHCID 552549(Trifluoromethyl)trimethylsilaneHCID 70066515-Bromo-2-iodopyrimidine

生成物 1

HCID 336979635-Bromo-2-(trifluoromethyl)pyrimidine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

実験手順

A mixture of potassium fluoride (1.77 g) and cuprous iodide (5.79 g) was stirred and heated together using a heat gun under vacuum (˜1 mm) for 20 min. After cooling, dimethyl formamide (20 ml) and N-methyl pyrrolidinone (20 ml) were added followed by (trifluoromethyl)trimethylsilane (4.1 ml) and 5-bromo-2-iodopyrimidine (6.5 g). The mixture was stirred at rt for 5 h and then the brown solution was poured into 6N ammonia solution. The product was extracted into ethyl acetate and the extracts were washed with sodium bicarbonate solution and brine and then dried (Na2SO4) and evaporated. Chromatography on silica gel (elution with 20-50% dichloromethane in pentane) gave the title compound (D30) as a white solid (2.4 g). 1H NMR (CDCl3): 8.97 (2H, s).

後処理

  1. temperatureheated together
  2. customfor 20 min
  3. temperatureAfter cooling
  4. stirringThe mixture was stirred at rt for 5 h
  5. extractionThe product was extracted into ethyl acetate
  6. washthe extracts were washed with sodium bicarbonate solution and brine
  7. dry with materialdried (Na2SO4)
  8. customevaporated

出典と根拠

ORDレコード
ord-8a3c2b0fa54640a5b372585a9998c897
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592347B2

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