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 14148373、化合物

HRID 247608
ノート
印刷プレビュー

反応式

HRID 247608 の反応式
CC(C)([O-])C.[Na+].[H-].[Na+].[C:9]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:14]=1[OH:23])([CH3:12])([CH3:11])[CH3:10].[CH2:24]([N:28]1[C:32](=[O:33])[CH:31]=[CH:30][C:29]1=[O:34])[CH2:25][CH2:26][CH3:27]>C(O)(C)(C)C.O.C(O)(=O)C>[C:19]([C:15]1[CH:16]=[C:17]([CH:31]2[CH2:30][C:29](=[O:34])[N:28]([CH2:24][CH2:25][CH2:26][CH3:27])[C:32]2=[O:33])[CH:18]=[C:13]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:14]=1[OH:23])([CH3:22])([CH3:21])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 314052,6-Di-tert-butylphenolHCID 239780N-ButylmaleimideHCID 23676156Sodium t-butoxide

生成物 1

HCID 14148373HCID 14148373、化合物収率 12%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒
HCID 962
Water
溶媒
HCID 6386tert-Butanol溶媒3 回

実験手順

To a solution of sodium tert-butoxide prepared from 2.40 g (0.1 mol) of sodium hydride and 135 ml of tert-butyl alcohol is added dropwise a solution of 20.63 g (0.1 mol) of 2,6-di-tert-butylphenol in 100 ml of tert-butyl alcohol. The reaction mixture is stirred at room temperature for 150 minutes and then to the resultant green solution is added dropwise over 120 minutes a solution of 15.31 g (0.1 mol.) of N-n-butylmaleimide in 50 ml of tert-butyl alcohol. The reaction mixture is stirred at room temperature overnight and is then mixed with 10 ml of glacial acetic acid. The reaction mixture is poured into 1.5 1 of water and the resultant mixture is extracted twice with chloroform. The organic extracts are combined and dried over anhydrous sodium sulfate. The solvent is removed in vacuo and the residue is purified by flash chromatography (3:1 heptane:toluene eluent) to give 4.25 g (12%) of a white solid: mp 109°-112° C.;

後処理

  1. stirringThe reaction mixture is stirred at room temperature overnight
  2. extractionthe resultant mixture is extracted twice with chloroform
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent is removed in vacuo
  5. customthe residue is purified by flash chromatography (3:1 heptane:toluene eluent)

出典と根拠

ORDレコード
ord-0ba0710192d5404fb69e4eb32706a858
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04709050

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