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

Methyl iodide → HCID 22097036、化合物

HRID 1458553
ノート
印刷プレビュー

反応式

HRID 1458553 の反応式
[CH3:1]C(C)([O-])C.[K+].[Cl:7][C:8]1[C:9]([NH:23][S:24]([CH2:27][CH3:28])(=[O:26])=[O:25])=[C:10]2[C:15](=[CH:16][C:17]=1[Cl:18])[N:14]=[C:13]([O:19][CH3:20])[C:12]([O:21][CH3:22])=[N:11]2.CI>CN(C)C=O>[Cl:7][C:8]1[C:9]([N:23]([CH3:1])[S:24]([CH2:27][CH3:28])(=[O:26])=[O:25])=[C:10]2[C:15](=[CH:16][C:17]=1[Cl:18])[N:14]=[C:13]([O:19][CH3:20])[C:12]([O:21][CH3:22])=[N:11]2
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 6328Methyl iodideHCID 22097009HCID 22097009、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 22097036HCID 22097036、化合物収率 79%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °C

実験手順

Potassium tert-butoxide (67.5 mg, 1.1 mmol) was added to a stirred solution of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)ethanesulphonamide (Preparation 4) (200 mg, 0.55 mmol) in dry dimethylformamide (3 ml) under nitrogen at 20° C. After 5 minutes, methyl iodide (38 μl, 1.1 mmol) was added and the mixture was stirred at 20° C. for 2 hours. The mixture was concentrated under reduced pressure, partitioned between ethyl acetate and water, and the combined organic extracts were washed with dilute aqueous sodium hydroxide. The solution was dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography (eluting with dichloromethane) to give N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(methyl)ethanesulphonamide (150 mg, 79%).

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. custompartitioned between ethyl acetate and water
  3. washthe combined organic extracts were washed with dilute aqueous sodium hydroxide
  4. dry with materialThe solution was dried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash chromatography (eluting with dichloromethane)

出典と根拠

ORDレコード
ord-a762b4163d8e413689e1ba08022c6ec5
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05852016

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