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

HRID 611640

반응식

HRID 611640 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178418371HCID 178418371, 화합물수율 77%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-40912572d58e484faf44f92324215029
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001863

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