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Water → 2-((3,4-Dihydro-2,2-dimethyl-4-phenyl-2H-1-benzopyran-7-yl)oxy)-N,N-dimethylethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Chloro-N,N-dimethylethylamine | HCID 7901 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,2-Dimethyl-7-hydroxy-4-phenylchroman | HCID 20570531 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-((3,4-Dihydro-2,2-dimethyl-4-phenyl-2H-1-benzopyran-7-yl)oxy)-N,N-dimethylethanamine | HCID 10428696 | — |
反応手順
A mixture of 2,2-dimethyl-7-hydroxy-4-phenylchroman (3.72 g), sodium hydride (0.53 g, 60% dispersion in oil) and 2-dimethylaminoethyl chloride (1.58 g) in toluene (59 ml) was stirred and boiled under reflux for 6 hours. Water was added to the cooled mixture and the organic layer was separated and extracted with 5N hydrochloric acid (3 × 30 ml). The combined acid extract was basified, extracted with ether and the ether extract dried (magnesium sulphate). Removal of the solvent gave 2,2-dimethyl-7-dimethylaminoethoxy-4-phenylchroman which was isolated as its hydrochloride salt, m.p. 165°-167° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04146539 |
| 出典データセット | uspto-grants-1979_03 |
| ORD ID | ord-7463360d25394477830da7721887bb44 |
| 出典メモ | uspto-grants-1979_03 |