Potassium Hydroxide → 8-Chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a] [1,4]benzodiazepin-1-thione-3-carboxylic acid

HRID 26048Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 26048
[OH-].[K+].C[O:4][C:5]([C:7]1[NH:8][C:9](=[S:29])[N:10]2[C:16]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:15]=3[C:14]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[Cl:28])=[N:13][CH2:12][C:11]=12)=[O:6]>CO>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]2[N:10]3[C:9](=[S:29])[NH:8][C:7]([C:5]([OH:6])=[O:4])=[C:11]3[CH2:12][N:13]=[C:14]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[Cl:28])[C:15]=2[CH:20]=1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 54335518HCID 54335518, Verbindung

Produkt 1

HCID 203945858-Chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a] [1,4]benzodiazepin-1-thione-3-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 1.1 g (0.02 mole) of potassium hydroxide in 40 ml of methanol was treated with 2.1 g (0.005 mole) of 8-chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-1-thione-3-carboxylic acid methyl ester in a beaker. The solution was boiled in a steambath for 15 min and then evaporated at reduced pressure at 50°-60°. An aqueous solution of the residue was acidified with cold 6N aqueous hydrochloric acid adding ice to keep the mixture cold. The solid was collected by filtration, washed with water and air dried on the funnel overnight to yield crude end product. Recrystallization from ethanol gave light tan crystals with mp 277°-280° (dec).

Aufarbeitung

  1. customevaporated at reduced pressure at 50°-60°
  2. additionadding ice
  3. filtrationThe solid was collected by filtration
  4. washwashed with water and air
  5. customdried on the funnel overnight
  6. customto yield crude end product
  7. customRecrystallization from ethanol
  8. customgave light tan crystals with mp 277°-280° (dec)

Quellen und Nachweise

ORD-Eintrag
ord-1092a4007c4c4eb49cab5fbe2165453d
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04147875

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