Methanol → trans-5-(4-Ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

HRID 1812

Reaktionsgleichung

Reaktionsgleichung von HRID 1812
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C@@H:10]2[C:16]3[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=3[N:14]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[C:13](=[O:27])[C@@H:12]([CH2:28][C:29]([O:31]CC)=[O:30])[O:11]2)=[C:6]([O:34][CH3:35])[CH:5]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].CO.O1CCCC1>O>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C@@H:10]2[C:16]3[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=3[N:14]([CH2:22][C:23]([CH3:25])([CH3:26])[CH3:24])[C:13](=[O:27])[C@@H:12]([CH2:28][C:29]([OH:31])=[O:30])[O:11]2)=[C:6]([O:34][CH3:35])[CH:5]=1)[CH3:2]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 67603127Ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

Produkt 1

HCID 10140397trans-5-(4-Ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (0.18 g), potassium carbonate (0.10 g), methanol (10 ml), tetrahydrofuran (10 ml) and water (5 ml) was refluxed for 1.5 h. The resulting mixture was concentrated in vacuo, acidified with 1N hydrochloric acid (50 ml) and extracted with ethyl acetate (50 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo to give trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid as colorless crystals (mp=230°-232° C.).

Aufarbeitung

  1. temperaturewas refluxed for 1.5 h
  2. concentrationThe resulting mixture was concentrated in vacuo
  3. extractionextracted with ethyl acetate (50 ml)
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-272d2516523f4474ab76d5851158b256
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05726306

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