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Hydrochloric Acid → 2-Tetrahydropyranylmethyl 2-(7-chloro-4-quinolyl)aminobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydropyran-2-methanol | HCID 7524 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Methyl 2-(7-trifluoromethyl-4-quinolyl)aminobenzoate | HCID 21294482 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diisopropyl Ether | HCID 7914 | — |
| 生成物 | 2-Tetrahydropyranylmethyl 2-(7-chloro-4-quinolyl)aminobenzoate | HCID 21294474 | 67% |
反応手順
By treating 15.4 g of methyl 2-(7-chloro-4-quinolyl)aminobenzoate (II, R=Cl, R"=CH3), 8.46 g of 2-hydroxymethyltetrahydropyran, 125 ml of toluene and in the presence of sodium, as described in Example 1, 19.8 g of a crude material are isolated. This material is dissolved in 250 ml of diisopropyl ether and 7 ml of hydrochloric acid (g) 10N ethanolic solution are added under cooling in water-ice bath. After 15 minutes the precipitated hydrochloride is filtered off, dried (19.45 g; 91%) and recrystallized in acetonitrile. 14.34 g (yield: 67%) of the hydrochloride--yellow solid--are obtained with m.p. 187°-187.5° C. and elemental analysis C, H, N, Cl correct.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04767767 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-358f88f48e804101b8422a64e4e175f2 |
| 出典メモ | uspto-grants-1988_08 |