Acryloyl chloride → 5-acryloyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

HRID 354788

Reaktionsgleichung

Reaktionsgleichung von HRID 354788
[CH:1]1[C:11]2[C:10](=[O:12])[NH:9][C:8]3[CH:13]=[CH:14][CH:15]=[CH:16][C:7]=3[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:17](Cl)(=[O:20])[CH:18]=[CH2:19]>C1(C)C=CC=CC=1>[C:17]([N:6]1[C:5]2[CH:4]=[CH:3][CH:2]=[CH:1][C:11]=2[C:10](=[O:12])[NH:9][C:8]2[CH:13]=[CH:14][CH:15]=[CH:16][C:7]1=2)(=[O:20])[CH:18]=[CH2:19]

Komponenten

4

Edukt 2

HCID 13140Acryloyl chlorideHCID 2013275,10-Dihydro-11H-dibenzo(b,e)(1,4)diazepin-11-one

Produkt 1

HCID 128347105-acryloyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

5.26 gm (0.025 mol) of 5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one and 2.7 gm (0.03 mol) of acrylic acid chloride were refluxed in 200 ml of toluene for 3 hours. Subsequently, the reaction mixture was evaporated in vacuo to dryness, and the residue was stirred with aqueous sodium bicarbonate solution. After suction-filtering, washing with water, and drying, 5-acryloyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one was obtained with a quantitative yield. Recrystallization from ethanol.

Aufarbeitung

  1. customSubsequently, the reaction mixture was evaporated in vacuo to dryness
  2. filtrationAfter suction-filtering
  3. washwashing with water
  4. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-f5d265f2e4324dbf8d597c9b9a53ee0f
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04377576

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