Methanol → Methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate

HRID 1679560Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1679560
[O:1]=[C:2]1[C:8]2[CH:9]=[C:10]([CH2:13][C:14]([OH:16])=[O:15])[CH:11]=[CH:12][C:7]=2[O:6][CH2:5][C:4]2[CH:17]=[CH:18][S:19][C:3]1=2.S(=O)(=O)(O)O.[CH3:25]O>>[O:1]=[C:2]1[C:8]2[CH:9]=[C:10]([CH2:13][C:14]([O:16][CH3:25])=[O:15])[CH:11]=[CH:12][C:7]=2[O:6][CH2:5][C:4]2[CH:17]=[CH:18][S:19][C:3]1=2

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 123447152-(10-oxo-4H-thieno[3,2-c][1]benzoxepin-8-yl)acetic acid

Produkt 1

HCID 13051081Methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate

Versuchsvorschrift

A mixture of 0.70 g of 4,10-dihydro-10-oxothieno-[3,2-c][1]benzoxepin-8-acetic acid (Example 1), 8 ml of concentrated sulfuric acid, and 150 ml of methanol is refluxed for 16 hours. The reaction mixture is concentrated in vacuo, diluted with water and extracted with benzene. The combined benzene extracts are washed with 5% sodium hydroxide and water, dried, filtered and concentrated in vacuo to an oil which solidifies upon standing. The solid is recrystallized from methanol to provide light yellow crystals, mp 80°-81° C. of methyl 4,10-dihydro-10-oxothieno[3,2-c][1]benzoxepin-8-acetate.

Aufarbeitung

  1. temperatureis refluxed for 16 hours
  2. concentrationThe reaction mixture is concentrated in vacuo
  3. additiondiluted with water
  4. extractionextracted with benzene
  5. washThe combined benzene extracts are washed with 5% sodium hydroxide and water
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo to an oil which
  9. customThe solid is recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-bc2f81739fbd46bb86fe5866049766c7
Quelldatensatz
uspto-grants-1978_03
Patentnummer
US04081457

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