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

HRID 2308937노트

반응식

HRID 2308937 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-64ee2668a0f64786bf28656156860fa4
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692444

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