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

Dimethylformamide → HCID 131716995、化合物

HRID 727792
ノート
印刷プレビュー

反応式

HRID 727792 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[C:14]3[CH:9]([CH2:10][C:11](=[O:21])[N:12]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=4)[N:13]=3)[CH2:8][CH2:7][C:6]=2[CH:22]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[Cl:34][CH2:35][CH2:36][CH2:37][N:38]1[CH2:43][CH2:42][O:41][CH2:40][CH2:39]1>O>[ClH:34].[ClH:34].[O:41]1[CH2:42][CH2:43][N:38]([CH2:37][CH2:36][CH2:35][O:1][C:2]2[CH:3]=[CH:4][C:5]3[C:14]4[CH:9]([CH2:10][C:11](=[O:21])[N:12]([C:15]5[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=5)[N:13]=4)[CH2:8][CH2:7][C:6]=3[CH:22]=2)[CH2:39][CH2:40]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 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 958344-(3-Chloropropyl)morpholineHCID 135816633HCID 135816633、化合物

生成物 1

HCID 131716995HCID 131716995、化合物収率 30.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
55 °C

実験手順

To a mixture of 1.4 g of 8-hydroxy-2-(2-pyridyl)-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one, 1.4 g of potassium carbonate and 30 ml of dimethylformamide is added 1.3 g of N-(3-chloropropyl)morpholine, and the mixture is stirred at 55° C. for 3 hours. After the completion of the reaction, water is added to the reaction mixture and the mixture is extracted with ethyl acetate. The extract is washed with water and dried over magnesium sulfate. The solvent is distilled off under reduced pressure. The obtained oily substance is purified by silica gel column chromatography (chloroform : methanol =10 : 1) and converted into the hydrochloride in methanol, which is recrystallized from methanol to give 0.6 g of 8-(3-morpholinopropoxy)-2-(2-pyridyl)-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one. dihydrochloride.dihydrate as white crystals, m.p. 201°-202° C. (decomposition).

後処理

  1. additionis added to the reaction mixture
  2. extractionthe mixture is extracted with ethyl acetate
  3. washThe extract is washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent is distilled off under reduced pressure
  6. customThe obtained oily substance is purified by silica gel column chromatography (chloroform : methanol =10 : 1)
  7. customis recrystallized from methanol

出典と根拠

ORDレコード
ord-7cffa23dfa6944f0861fcf7c37eb8a1c
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05045541

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