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

HRID 1904231노트

반응식

HRID 1904231 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 75 ml of ethanol were added 17.0 g (0.085 mol) of 2-t-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 reflax 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, dried over anhydrous sodium sulfate and then freed of solvent by distillation to obtain 16.3 g of a crude product.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with 200 ml of ethyl ether
  3. washThe ether layer was washed with 100 ml of water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationfreed of solvent by distillation

출처 및 근거

ORD 기록
ord-a7b87b1a982d44db8a19ec7c8a410a02
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04837217

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