Acetic Acid → 8-Chloro-2,4-dihydrothiochromeno[4,3-C]pyrazole

HRID 2308937ノート

反応式

HRID 2308937 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8](=[CH:11][N:12](C)C)[C:7](=O)[C:6]=2[CH:16]=1.O.[NH2:18]N.C(O)(=O)C>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8]3[CH:11]=[N:12][NH:18][C:7]=3[C:6]=2[CH:16]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 38135366-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

生成物 1

HCID 27396788-Chloro-2,4-dihydrothiochromeno[4,3-C]pyrazole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one (7 g), hydrazine hydrate (2.01 ml), and acetic acid (2.37 ml) in methanol (140 ml) was stirred at room temperature for 5 hours and then evaporated in vacuo. To the residue was added aqueous sodium bicarbonate and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue solid was recrystallized from ethyl acetate to give 8-chloro-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole (2.85 g).

後処理

  1. customevaporated in vacuo
  2. additionTo the residue was added aqueous sodium bicarbonate
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue solid was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-64ee2668a0f64786bf28656156860fa4
出典データセット
uspto-grants-1987_09
特許番号
US04692444

反応ノート

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