Diethylamine → Benzo[b][1,4]thiazepin-4(5H)-one, 2,3-dihydro-3-acetoxy-2-(4-methoxyphenyl)-

HRID 1649328Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1649328
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH:15]([O:16][C:17](=[O:19])[CH3:18])[C:14](=[O:20])[N:13](C(=O)C)[C:12]3[CH:24]=[CH:25][CH:26]=[CH:27][C:11]=3[S:10]2)=[CH:5][CH:4]=1.C(NCC)C>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]2[CH:15]([O:16][C:17](=[O:19])[CH3:18])[C:14](=[O:20])[NH:13][C:12]3[CH:24]=[CH:25][CH:26]=[CH:27][C:11]=3[S:10]2)=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 8021DiethylamineHCID 132366692-(4'-Methoxyphenyl)-3-acetoxy-5-acetyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one2×

Produkt 1

HCID 591255Benzo[b][1,4]thiazepin-4(5H)-one, 2,3-dihydro-3-acetoxy-2-(4-methoxyphenyl)-Ausbeute 94,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

7-(1). 2-(4'-Methoxyphenyl)-3-acetoxy-5-acetyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one [Compound (VII)] (1.93 g) and diethylamine (0.44 g) are added to chloroform (20 ml), and the mixture is stirred at room temperature for one hour. After distilling off chloroform, water is added to the residue, and the precipitated crystals are separated by filtration, washed with water and dried to give the title compound (II) (1.63 g, 94.8%), m.p. 198°-200° C.

Aufarbeitung

  1. distillationAfter distilling off chloroform, water
  2. additionis added to the residue
  3. customthe precipitated crystals are separated by filtration
  4. washwashed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-55ea379747b34aa6b34df4dfe3a62e1b
Quelldatensatz
uspto-grants-1983_11
Patentnummer
US04416819

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