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

Sodium hydride → HCID 57086818、化合物

HRID 278376
ノート
印刷プレビュー

反応式

HRID 278376 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[N:15][O:16][CH3:17])[C:11]([NH:13][CH3:14])=[O:12].[Cl:18][C:19]1[CH:33]=[CH:32][CH:31]=[CH:30][C:20]=1[O:21][C:22]1[C:27]([F:28])=[C:26](F)[N:25]=[CH:24][N:23]=1>CN(C)C=O>[Cl:18][C:19]1[CH:33]=[CH:32][CH:31]=[CH:30][C:20]=1[O:21][C:22]1[N:23]=[CH:24][N:25]=[C:26]([O:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:10](=[N:15][O:16][CH3:17])[C:11]([NH:13][CH3:14])=[O:12])[C:27]=1[F:28]
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

5

反応物 3

HCID 24758Sodium hydrideHCID 110538434-(2-Chlorophenoxy)-5,6-difluoropyrimidineHCID 136045378N-methyl-2-(2-hydroxyphenyl)-2-methoxyiminoacetamide

生成物 1

HCID 57086818HCID 57086818、化合物収率 51.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
25 °C

実験手順

With cooling, 0.4 g (0.01 mol) of sodium hydride (60%) are added to a mixture of 2 g (0.0096 mol) of 2-(2-hydroxy-phenyl)-2-methoxyimino-N-methyl-acetamide and 2.3 g (0.0095 mol) of 4-(2-chlorophenoxy)-5,6-difluoropyrimidine in 10 ml of dimethylformamide, and the mixture is stirred at 25° C. for 12 hours. The reaction mixture is poured onto water and extracted with dichloromethane, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. The residue is chromatographed over silica gel using a mixture of identical volumina of ethyl acetate and cyclohexane. 2.1 g (48.3% of theory) of 2-{2-[6-(2-chlorophenoxy)-5-fluoro-pyrimidine4-yloxy]-phenyl}-2-methoxyimino-N-methylacetamide are obtained.

後処理

  1. temperatureWith cooling
  2. additionThe reaction mixture is poured onto water
  3. extractionextracted with dichloromethane
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue is chromatographed over silica gel using
  7. additiona mixture of identical volumina of ethyl acetate and cyclohexane

出典と根拠

ORDレコード
ord-0c40044984e24ba8aa3344fd492e52e0
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06359133B2

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