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

Diisopropylethylamine → HCID 23377662、化合物

HRID 1066748
ノート
印刷プレビュー

反応式

HRID 1066748 の反応式
[CH3:1][O:2][CH2:3][CH:4]([NH2:9])[CH2:5][CH2:6][O:7][CH3:8].Cl[C:11]1[CH:16]=[C:15]([CH3:17])[NH:14][C:13](=[O:18])[C:12]=1[N+:19]([O-:21])=[O:20].C(N(C(C)C)CC)(C)C>CC#N.C(Cl)Cl>[CH3:17][C:15]1[NH:14][C:13](=[O:18])[C:12]([N+:19]([O-:21])=[O:20])=[C:11]([NH:9][C@H:4]([CH2:3][O:2][CH3:1])[CH2:5][CH2:6][O:7][CH3:8])[CH:16]=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

6

反応物 3

HCID 81531DiisopropylethylamineHCID 114354124-Chloro-6-methyl-3-nitropyridin-2(1H)-oneHCID 18629275HCID 18629275、化合物

生成物 1

HCID 23377662HCID 23377662、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

1-methoxymethyl-3-methoxypropylamine (4.19 g, 22.3 mmol), and 4-chloro-6-methyl-3-nitropyridone (3.87 g, 22.3 mmol) were mixed in CH3CN (70 mL) and diisopropyl- ethylamine (9.4 mL, 53.6 mmol) was added. The reaction was stirred at 25° C. for 16 h and at reflux for 2.5 h. The solvent was stripped off and the residue was dissolved in CH2Cl2 (150 mL) and the CH2Cl2 was washed with water (80 mL). The water was extracted with CH2Cl2 (50 mL) and the combined organic extracts were dried (MgSO4) and stripped in vacuo. The residue was crystallized from EtOAc and washed with 40% EtOAc/hexanes to give the product, (4.8 g, 75%).

後処理

  1. temperatureat reflux for 2.5 h
  2. washthe CH2Cl2 was washed with water (80 mL)
  3. extractionThe water was extracted with CH2Cl2 (50 mL)
  4. dry with materialthe combined organic extracts were dried (MgSO4)
  5. customThe residue was crystallized from EtOAc
  6. washwashed with 40% EtOAc/hexanes
  7. customto give the product, (4.8 g, 75%)

出典と根拠

ORDレコード
ord-794e873e5cab4b14b28153ff640f4831
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06245769B1

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