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Ethylene Oxide → 10-chloro-11b-phenyl-2,3,5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6(7H)-one-5-carboxylic acid ethyl ester

HRID 2071948
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2071948
[CH2:1]([O:3][C:4]([CH:6]1[N:12]=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:10]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:9]=2[NH:8][C:7]1=[O:24])=[O:5])[CH3:2].[CH2:25]1[O:27][CH2:26]1.[OH-].[NH4+]>C(Cl)CCl>[CH2:1]([O:3][C:4]([CH:6]1[N:12]2[CH2:25][CH2:26][O:27][C:11]2([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:10]2[CH:19]=[C:20]([Cl:23])[CH:21]=[CH:22][C:9]=2[NH:8][C:7]1=[O:24])=[O:5])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6354Ethylene OxideHCID 14923Ammonium HydroxideHCID 110682Ethyl 7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylate

Produkt 1

HCID 5391709210-chloro-11b-phenyl-2,3,5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6(7H)-one-5-carboxylic acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11
1,2-Dichloroethane
Lösungsmittel
2×

Versuchsvorschrift

To a solution of 3.1 g. (0.0118 M) of stannic chloride in 35 ml. of dry ethylene dichloride under nitrogen was added 1.5 g. (0.00438 M) of 7-chloro-1,3-dihydro-2-oxo-5-phenyl-2H-1,4-benzodiazepine-3-carboxylic acid ethyl ester. The reaction was stirred in an ice bath, when a solution of 1.0 g. (0.0233 M) of ethylene oxide in 5 ml. of ethylene dichloride was added. The mixture was stirred at room temperature for 3 hr. and then made basic with mixture of ammonium hydroxide and ice. The mixture was filtered, and the filtrate was dried with anhydrous sodium sulfate and evaporated to dryness. The residue was crystallized from ether. Recrystallization from a mixture of dichloromethane and petroleum ether gave 10-chloro-11b-phenyl-2,3,5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6(7H)-one-5-carboxylic acid ethyl ester as white rods, m.p. 205°-207°.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 3 hr
  2. filtrationThe mixture was filtered
  3. dry with materialthe filtrate was dried with anhydrous sodium sulfate
  4. customevaporated to dryness
  5. customThe residue was crystallized from ether
  6. customRecrystallization
  7. additionfrom a mixture of dichloromethane and petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-40fe3507cdd2417e98cf419bc3aa84ef
Quelldatensatz
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04049667

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