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

HRID 2352013ノート

反応式

HRID 2352013 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ea6e550985fa4ef7a3b733fbe95e7ea3
出典データセット
uspto-grants-1989_10
特許番号
US04874861

反応ノート

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