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

HRID 1904231ノート

反応式

HRID 1904231 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 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.

後処理

  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

出典と根拠

ORDレコード
ord-a7b87b1a982d44db8a19ec7c8a410a02
出典データセット
uspto-grants-1989_06
特許番号
US04837217

反応ノート

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