HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 9-chloro-7-(2-chlorophenyl)-2-isopropyl-5H-pyrimido[5,4-d][2]benzazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | 2-Methylpropanimidamide hydrochloride | HCID 2782053 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Edukt | 1-(2-Chlorophenyl)-3,4-dihydro-4-[(dimethylamino)methylene]-5H-2-benzazepin-5-one | HCID 53826441 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 9-chloro-7-(2-chlorophenyl)-2-isopropyl-5H-pyrimido[5,4-d][2]benzazepine | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04546183 |
| Quelldatensatz | uspto-grants-1985_10 |
| ORD ID | ord-9d2786fe2a534bda928b15b27a668123 |
| Quellennotiz | uspto-grants-1985_10 |