Hydrochloric Acid → 8-Chloro-1-methyl-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole

HRID 2308940노트

반응식

HRID 2308940 반응식
Cl.C(O[C:7]([N:9](C)[NH:10][CH:11]=[C:12]1[C:17](=O)[C:16]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:15]=2[S:14][CH2:13]1)=O)(C)(C)C>CO>[Cl:23][C:20]1[CH:21]=[CH:22][C:15]2[S:14][CH2:13][C:12]3[CH:11]=[N:10][N:9]([CH3:7])[C:17]=3[C:16]=2[CH:19]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 53870822HCID 53870822, 화합물

생성물 1

HCID 201864418-Chloro-1-methyl-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole수율 73.7%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of hydrogen chloride in methanol (225 ml) was added to a suspension of 3-(2-t-butoxycarbonyl-2-methylhydrazinomethylene)-6-chloro-2,3-dihydro-4H-1-benzothiopyran-4-one (54.14 g) in methanol (550 ml). After being stirred at ambient temperature for 8 hours, the mixture was evaporated in vacuo and the residue was extracted with ethyl acetate after an addition of water. The extract was washed with aqueous sodium bicarbonate and then water, dried over magnesium sulfate, and evaporated in vacuo to give 8-chloro-1-methyl-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole (26.63 g).

후처리

  1. customthe mixture was evaporated in vacuo
  2. extractionthe residue was extracted with ethyl acetate
  3. additionafter an addition of water
  4. washThe extract was washed with aqueous sodium bicarbonate
  5. dry with materialwater, dried over magnesium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-fa65e1bdc7fa4b1ea536b81d587d3b25
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692444

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