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

2,2,2-Trifluoroethanol → 1-[2-(2,2,2-Trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine

HRID 22213
ノート
印刷プレビュー

反応式

HRID 22213 の反応式
[H-].[Na+].[F:3][C:4]([F:8])([F:7])[CH2:5][OH:6].[H][H].[Na].FC(F)(F)CO.Cl[C:19]1[CH:24]=[CH:23][C:22]([CH2:25][N:26]2[CH2:30][CH2:29][NH:28][C:27]2=[N:31][N+:32]([O-:34])=[O:33])=[CH:21][N:20]=1>C1(C)C=CC=CC=1.CN(C)C1C=CN=CC=1>[F:3][C:4]([F:8])([F:7])[CH2:5][O:6][C:19]1[CH:24]=[CH:23][C:22]([CH2:25][N:26]2[CH2:30][CH2:29][NH:28][C:27]2=[N:31][N+:32]([O-:34])=[O:33])=[CH:21][N:20]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 867421422,2,2-Trifluoroethanol sodium saltHCID 1355277641-[(6-chloropyridin-3-yl)methyl]-N-nitroimidazolidin-2-imineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 1363427901-[2-(2,2,2-Trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine
収率 23.6%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

Sodium hydride (0.48 g) was added to a solution of 2,2,2-trifluoroethanol (2.4 g) in toluene (30 ml) was added, and the mixture was stirred until the generation of hydrogen ceased. As a result, 2,2,2-trifluoroethanol sodium salt was prepared. To the product were added 1-(2-chloro-5-pyridylmethyl)-2-(nitroimino)imidazolidine (5.1 g) synthesized by the method of Example 3 and a catalytic amount of 4-dimethylaminopyridine. The mixture was heated at 80° C. for 10 hours with stirring. After cooling the reaction mixture, the precipitated crystals were collected by filtration, washed with water and ether and then purified by silica gel chromatography to give 1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine (1.5 g).

後処理

  1. additionwas added
  2. customsynthesized by the method of Example 3
  3. temperatureAfter cooling the reaction mixture
  4. filtrationthe precipitated crystals were collected by filtration
  5. washwashed with water and ether
  6. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-37f501ed7b344cf2b37eaf2f0fd15b97
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05428032

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート