Acetic Anhydride → HCID 10554645, Verbindung

HRID 1981936Notizen

Reaktionsgleichung

[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@H:9]2[C@@H:15]([OH:16])[C:14](=[O:17])[N:13]([CH2:18][CH2:19][N:20]([C:22]([O:24][CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[O:23])[CH3:21])[C:12]3[CH:32]=[CH:33][C:34]([CH3:36])=[CH:35][C:11]=3[S:10]2)=[CH:5][CH:4]=1.[C:37](OC(=O)C)(=[O:39])[CH3:38]>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C@H:9]2[C@@H:15]([O:16][C:37](=[O:39])[CH3:38])[C:14](=[O:17])[N:13]([CH2:18][CH2:19][N:20]([C:22]([O:24][CH2:25][C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)=[O:23])[CH3:21])[C:12]3[CH:32]=[CH:33][C:34]([CH3:36])=[CH:35][C:11]=3[S:10]2)=[CH:7][CH:8]=1

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

A mixture of 2.49 g of (±)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-benzyloxycarbonyl-N-methylamino)ethyl]-8-methyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 15 ml of acetic anhydride and 5 ml of pyridine is stirred at 100° C. for 2 hours. The mixture is evaporated under reduced pressure to remove acetic anhydride and pyridine. Toluene is added to the residue, and the mixture is evaporated under reduced pressure to remove solvent (This operation is repeated again). 3.08 g of (±)-cis-2-(4-methoxyphenyl)-3-acetoxy-5-[2-(N-benzyloxycarbonyl-N-methylamino)ethyl]-8-methyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained as an oil.

Aufarbeitung

customThe mixture is evaporated under reduced pressure
customto remove acetic anhydride and pyridine
additionToluene is added to the residue
customthe mixture is evaporated under reduced pressure
customto remove solvent (This operation

Quellen und Nachweise

ORD-Eintrag: ord-7e2ec0a503c14f9cad8c5531c64e14f2
Quelldatensatz: uspto-grants-1986_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04594342

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