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

Carbon Disulfide → 6-(3-Isothiocyanatopropoxy)carbostyril

HRID 2257901
ノート
印刷プレビュー

反応式

HRID 2257901 の反応式
Cl.[NH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2.[C:18](=S)=[S:19].[OH-].[Na+].C(Cl)(=O)OCC>O>[N:2]([CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2)=[C:18]=[S:19]
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 6348Carbon DisulfideHCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 114141486-(3-aminopropoxy)-1H-quinolin-2-one;hydrochloride

生成物 1

HCID 229236916-(3-Isothiocyanatopropoxy)carbostyril収率 21.4%

試薬・触媒・溶媒 1

HCID 962Water
溶媒

反応条件

温度
80 °C

実験手順

1.28 g of 6-(3-aminopropoxy)carbostyril hydrochloride was added, at 0° C., to 10 ml of an aqueous solution containing 0.3 g of carbon disulfide and 0.4 g of sodium hydroxide. The mixture was stirred at 80° C. for about 2 hours. Thereto was added 0.55 g of ethyl chlorocarbonate at 35° C. The resulting mixture was stirred for 30 minutes. The reaction mixture was poured into water, followed by extraction with ethyl acetate. The filtrate was dried with magnesium sulfate. The solvent was removed by distillation. To the resulting residue was added diethyl ether, and the resulting crystals were collected by filtration and purified by a silica gel column chromatography (eluant: 3.3% methanol/dichloromethane) to obtain 0.22 g of 6-(3-isothiocyanatopropoxy)carbostyril.

後処理

  1. stirringThe resulting mixture was stirred for 30 minutes
  2. extractionfollowed by extraction with ethyl acetate
  3. dry with materialThe filtrate was dried with magnesium sulfate
  4. customThe solvent was removed by distillation
  5. additionTo the resulting residue was added diethyl ether
  6. filtrationthe resulting crystals were collected by filtration
  7. custompurified by a silica gel column chromatography (eluant: 3.3% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-5330a9fa9cdf4aefb3d4a8d43ebf7875
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05658926

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