Hydrazine hydrate (1:1) → HCID 18610546, Verbindung
Reaktionsgleichung
O.NN.[O:4]=[C:5]1[C@@H:11]([N:12]2C(=O)C3=CC=CC=C3C2=O)[CH2:10][S:9][CH:8]([C:23]2[S:24][CH:25]=[CH:26][CH:27]=2)[CH2:7][N:6]1[CH2:28][C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30]>CO>[NH2:12][C@H:11]1[CH2:10][S:9][CH:8]([C:23]2[S:24][CH:25]=[CH:26][CH:27]=2)[CH2:7][N:6]([CH2:28][C:29]([O:31][C:32]([CH3:34])([CH3:33])[CH3:35])=[O:30])[C:5]1=[O:4]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
7 ml of hydrazine hydrate were added to a suspension of 34.1 g of t-butyl α-[5-oxo-6(R)-phthalimido-2-(2-thienyl)perhydro-1,4-thiazepin-4-yl]acetate [prepared as described in step (f) above] in 340 ml of methanol, to form a homogeneous solution. This was left standing for 2 days at room temperature, and then the resulting precipitate was filtered off. The filtrate was condensed by evaporation under reduced pressure, and then 200 ml of methylene chloride were added to the residue. The mixture was stirred and insoluble matter was filtered off. The filtrate was washed with water and dried over anhydrous magnesium sulfate, after which the solvent was evaporated off. The residue was crystallized by adding diisopropyl ether containing a small amount of hexane, to yield 22.3 g of the title compound, melting at 81°-82° C.