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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 464168Erstellt: 26. Oktober 2026

Methanol → 9-chloro-7-(2-chlorophenyl)-2-isopropyl-5H-pyrimido[5,4-d][2]benzazepine

https://huagongshe.com/reaction/464168

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktMethanolHCID 887—
Edukt2-Methylpropanimidamide hydrochlorideHCID 2782053—
EduktSodium MethoxideHCID 10942334—
Edukt1-(2-Chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-oneHCID 53826441—
LösungsmittelWaterHCID 962—
Produkt9-chloro-7-(2-chlorophenyl)-2-isopropyl-5H-pyrimido[5,4-d][2]benzazepineHCID 13225506—

Reaktionsschritte

A mixture of 3.5 g (10 mmole) of 1-(2-chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one, 4.8 g (40 mmole) of isobutyramidine hydrochloride, 10 ml (41 mmole) of a 4.12M methanol solution of sodium methoxide and 100 ml of methanol was stirred at room temperature for 2 hr. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a yellow oil. Crystallization of the oil with ether gave a light yellow solid, mp 127°-129° C. Recrystallization from a mixture of ether and petroleum ether gave colorless rods, mp 127°-129° C.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS04546183
Quelldatensatzuspto-grants-1985_10
ORD IDord-9d2786fe2a534bda928b15b27a668123
Quellennotizuspto-grants-1985_10