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Methyl iodide → 7-chloro-4,5-dihydro-3-(3-methoxy-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]-benzodiazepin-6-one

HRID 1606993
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1606993
[OH-].[K+].[Cl:3][C:4]1[C:9]2[C:10](=[O:24])[N:11]([CH3:23])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH:20]([OH:22])[CH3:21])[C:8]=2[CH:7]=[CH:6][CH:5]=1.[CH3:25]I>CN(C)C=O>[Cl:3][C:4]1[C:9]2[C:10](=[O:24])[N:11]([CH3:23])[CH2:12][C:13]3[N:14]([CH:15]=[N:16][C:17]=3[C:18]#[C:19][CH:20]([O:22][CH3:25])[CH3:21])[C:8]=2[CH:7]=[CH:6][CH:5]=1
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Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 198306467-chloro-4,5-dihydro-3-(3-hydroxy-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

Produkt 1

HCID 198515487-chloro-4,5-dihydro-3-(3-methoxy-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]-benzodiazepin-6-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

4.0 g (69.5 mmol) of freshly powdered potassium hydroxide was stirred for 10 minutes in 40 ml of N,N-dimethylformamide and cooled to 10°. 5.48 g (17.3 mmol) of 7-chloro-4,5-dihydro-3-(3-hydroxy-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one and 4.94 g (35 mmol) of methyl iodide were added thereto in succession, the ice-bath was removed and the mixture was stirred for a further 1 hour. The reaction mixture was poured into 200 ml of water and extracted five times with methylene chloride. The combined organic extracts were washed four times with water, dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate there was obtained 7-chloro-4,5-dihydro-3-(3-methoxy-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]-benzodiazepin-6-one of melting point 139°-141°.

Aufarbeitung

  1. temperaturecooled to 10°
  2. customin succession, the ice-bath was removed
  3. additionThe reaction mixture was poured into 200 ml of water
  4. extractionextracted five times with methylene chloride
  5. washThe combined organic extracts were washed four times with water
  6. dry with materialdried over magnesium sulphate
  7. customevaporated
  8. customAfter recrystallization of the residue from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-d7fd4b0c697b46bf993295cf6f4d5c40
Quelldatensatz
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04863920

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