Water → 9-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

HRID 1681837Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1681837
[OH:1][CH2:2][CH2:3][C:4]1[S:18][C:7]2[S:8][CH2:9][CH2:10][CH:11]3[CH2:16][C:15](=[O:17])[NH:14][N:13]=[C:12]3[C:6]=2[CH:5]=1.C(N(CC)CC)C.[C:26](OC(=O)C)(=[O:28])[CH3:27].O>C1(C)C=CC=CC=1>[C:26]([O:1][CH2:2][CH2:3][C:4]1[S:18][C:7]2[S:8][CH2:9][CH2:10][CH:11]3[CH2:16][C:15](=[O:17])[NH:14][N:13]=[C:12]3[C:6]=2[CH:5]=1)(=[O:28])[CH3:27]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 190168139-(2-hydroxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

Produkt 1

HCID 190168369-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 1.0 g of 9-(2-hydroxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one, 2 ml of triethylamine and 2 ml of acetic anhydride in 20 ml of toluene is kept on a water bath at 80°-85° C. for 3 hours. After cooling, to the mixture is added water, the organic layer is collected by a separatory funnel and concentrated. To the residue is added hexane and the precipitated crystals are collected by filtration. The resulting crystals are recrystallized from isopropyl ether to give 0.5 g of 9-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one as white crystals, melting at 106°-108° C.

Aufarbeitung

  1. temperatureAfter cooling, to the mixture
  2. customthe organic layer is collected by a separatory funnel
  3. concentrationconcentrated
  4. additionTo the residue is added hexane
  5. filtrationthe precipitated crystals are collected by filtration
  6. customThe resulting crystals are recrystallized from isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-e378d3ca9f7542fc9cf3e0c3735183dc
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05175162

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