Sodium hydrosulfide → 2-t-butyl-5-mercapto-4-methyl-3(2H)-pyridazinone

HRID 2352013노트

반응식

HRID 2352013 반응식
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8](Cl)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[SH-:14].[Na+]>C(O)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH3:12])=[C:8]([SH:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 28015Sodium hydrosulfideHCID 138222642-tert-butyl-5-chloro-4-methylpyridazin-3-(2H)-one

생성물 1

HCID 138222652-t-butyl-5-mercapto-4-methyl-3(2H)-pyridazinone수율 96.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 75ml of ethanol were added 17.0 g (0.085 mol) of 2-tert.-butyl-5-chloro-4-methyl-3(2H)-pyridazinone and 8.5 g (0.106 mol) of 70% sodium hydrosulfide, and the mixture was stirred under reflux for 4 hours. After cooling, the mixture was poured into 300 ml of ice-water and extracted with 200 ml of ethyl ether. The ether layer was washed with 100 ml of water and dried over anhydrous sodium sulfate. The solvent was then distilled off therefrom to give 16.3 g of a crude product.

후처리

  1. temperatureunder reflux for 4 hours
  2. temperatureAfter cooling
  3. extractionextracted with 200 ml of ethyl ether
  4. washThe ether layer was washed with 100 ml of water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was then distilled off

출처 및 근거

ORD 기록
ord-ea6e550985fa4ef7a3b733fbe95e7ea3
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04874861

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