Acetic Acid → HCID 53870822, 화합물

HRID 2308939노트

반응식

HRID 2308939 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:15])[C:6]=2[CH:16]=1.[C:17]([O:21][C:22]([N:24]([CH3:26])N)=[O:23])([CH3:20])([CH3:19])[CH3:18].C(O)(=O)C>CO.O1CCCC1>[C:17]([O:21][C:22]([N:24]([CH3:26])[NH:12][CH:11]=[C:8]1[C:7](=[O:15])[C:6]2[CH:16]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[S:10][CH2:9]1)=[O:23])([CH3:20])([CH3:19])[CH3:18]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 37482801-Boc-1-methylhydrazineHCID 38135366-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one

생성물 1

HCID 53870822HCID 53870822, 화합물수율 129.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 6-chloro-2,3-dihydro-3-dimethylaminomethylene-4H-1-benzothiopyran-4-one (34.13 g), 1-t-butoxycarbonyl-1-methylhydrazine (59.14 g), and acetic acid (23.14 ml) in methanol (2 l) and tetrahydrofuran (1 l) was stirred at ambient temperature for 6 hours and then evaporated in vacuo. To the residue was added aqueous sodium bicarbonate and the mixture was extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo to give 3-(2-t-butoxycarbonyl-2-methylhydrazinomethylene)-6-chloro-2,3-dihydro-4H-1-benzothiopyran-4-one (61.65 g).

후처리

  1. customevaporated in vacuo
  2. additionTo the residue was added aqueous sodium bicarbonate
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-ad84993324b04b359da9ebb6f3715884
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692444

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