Acetic Acid → HCID 53870822, Verbindung

HRID 2308939Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2308939
[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]

Komponenten

6

Edukt 3

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

Produkt 1

HCID 53870822HCID 53870822, VerbindungAusbeute 129,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-ad84993324b04b359da9ebb6f3715884
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04692444

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