8-Chloro-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2yl-ethyl)-amide → HCID 178418371、化合物

HRID 53674

反応式

HRID 53674 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][CH2:8][NH:9][C:10]([C:12]1[CH:13]=[N:14][C:15]2[CH:16]=[C:17]3[O:25][CH2:24][O:23][C:18]3=[CH:19][C:20]=2[C:21]=1Cl)=[O:11].[SH2:26].[Na]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][CH2:8][NH:9][C:10]([C:12]1[CH:13]=[N:14][C:15]2[CH:16]=[C:17]3[O:25][CH2:24][O:23][C:18]3=[CH:19][C:20]=2[C:21]=1[SH:26])=[O:11]

参加物

4

反応物 2

HCID 571273518-Chloro-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2yl-ethyl)-amideHCID 86586439Sodium hydrogen sulphide

生成物 1

HCID 178418371HCID 178418371、化合物収率 77%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 10.4 g (0.025 mol) of 8-chloro-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2yl-ethyl)-amide in 100 mL of ethanol was added 7.2 g (0.1 mol) of sodium hydrogensulfide and the mixture was heated at reflux for 3 hours. The mixture was cooled and the solids filtered, washed with ethanol, and then with water. The filtrate was concentrated and the solids were suspended in water, collected by filtration, and recrystallized from ethanol to give 6.8 g of the title compound, mp 258°-260° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe mixture was cooled
  4. filtrationthe solids filtered
  5. washwashed with ethanol
  6. concentrationThe filtrate was concentrated
  7. filtrationcollected by filtration
  8. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-0ed0d8267f014d718d60bf3f5afeb68b
出典データセット
uspto-grants-1997_04
特許番号
US05620997

関連ノート

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