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4-Chloro-N-methylbenzenamine → Hydrochloric Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-N-methylbenzenamine | HCID 70272 | — |
| 反応物 | 4,7-Dichloroquinazoline | HCID 241881 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 7-Chloro-4-(4'-chloro-N-methylanilino)quinazoline | HCID 12774517 | — |
反応手順
2.5 g of 4,7-dichloroquinazoline and 2.2 g of p-chloro-N-methylaniline were added to 10 ml of ethanol and then the mixture was heated. The mixture became a homogeneous solution which solidified soon after. After cooling, the solidified crystals were collected and recrystallized from ethanol to give the desired compound in the form of its hydrochloride (Compound No. 68). The crystals of hydrochloride were crushed and added to a dilute aqueous solution of sodium hydroxide, with stirring, to precipitate the free base. The precipitate was collected by filtration, washed with water and recrystallized from ethanol to give 2.4 g (yield 65%) of the desired Compound No. 67 in the form of colourless plates melting at 129°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04464375 |
| 出典データセット | uspto-grants-1984_08 |
| ORD ID | ord-eb6788864d8246b19c761fdf5d1dd535 |
| 出典メモ | uspto-grants-1984_08 |