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

Hydrochloric Acid → HCID 14535921、化合物

HRID 1904911
ノート
印刷プレビュー

反応式

HRID 1904911 の反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:21]=[CH:20][C:8]([C:9]([C:11]2[CH:19]=[CH:18][CH:17]=[C:16]3[C:12]=2[CH:13]=[CH:14][NH:15]3)=[O:10])=[CH:7][CH:6]=1.[Cl:22][CH2:23][CH2:24][N:25]1[CH2:30][CH2:29][O:28][CH2:27][CH2:26]1.Cl>CCCCCC.CN(C=O)C.COC(C)(C)C.C(=O)(O)[O-].[Na+].C(OCC)(=O)C.O>[ClH:22].[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([C:9]([C:11]2[CH:19]=[CH:18][CH:17]=[C:16]3[C:12]=2[CH:13]=[CH:14][N:15]3[CH2:23][CH2:24][N:25]2[CH2:30][CH2:29][O:28][CH2:27][CH2:26]2)=[O:10])=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 4

HCID 313Hydrochloric Acid2 回HCID 24758Sodium hydrideHCID 767274-(2-Chloroethyl)morpholineHCID 14535919HCID 14535919、化合物

生成物 1

HCID 14535921HCID 14535921、化合物収率 70.2%

試薬・触媒・溶媒 6

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒
HCID 15413tert-Butyl methyl ether溶媒
HCID 516892Sodium Bicarbonate溶媒

実験手順

To a stirred mixture of 3.5 g (0.0887 mole) of a 60% suspension of sodium hydride in hexane in 50 ml of DMF was added 18.1 g (0.0721 mole) of 4-(4-methoxybenzoyl)indole. The mixture was then treated with a solution containing 0.18 mole of 4-(2-chloroethyl)morpholine in t-butyl methyl ether (prepared by extraction of the free base from a suspension of 35.5 g of the corresponding hydrochloride in saturated sodium bicarbonate). When addition was complete, the reaction mixture was heated under reflux for about twelve hours, treated with 1500 ml of water and extracted with 500 ml of ethyl acetate. The combined organic extracts, on drying and evaporation to dryness, afforded an oil which was dissolved in 250 ml of ethyl acetate and treated with 50 ml of ethereal hydrogen chloride. The material which separated was collected and recrystallized from ethanol to give 20.3 g of 4-(4-methoxybenzoyl)-1-[2-(4-morpholinyl)ethyl]-1H-indole hydrochloride, m.p. 177°-180° C.

後処理

  1. additionThe mixture was then treated with a solution
  2. additionWhen addition
  3. temperaturethe reaction mixture was heated
  4. temperatureunder reflux for about twelve hours
  5. extractionextracted with 500 ml of ethyl acetate
  6. customThe combined organic extracts, on drying
  7. customevaporation to dryness
  8. customafforded an oil which
  9. customThe material which separated
  10. customwas collected
  11. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-dae630c60d77452792356fb6f4120239
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04840950

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