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Phosgene → 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Benzhydryl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 11728694 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 19799606 | 62% |
反応手順
A solution of 35.6 g (0.36 mole) of phosgene in 200 ml of methylene chloride at 5° C. was stirred with 50 g (0.36 mole) of potassium carbonate for 1 hr. To the mixture was added dropwise 115 g (0.3 mole) of 1-diphenylmethyl-3-[-3-(trifluoromethyl)phenoxy]azetidine in 400 ml of methylene chloride. After stirring for 18 hr, the reaction mixture was filtered and the filtrate was washed with water, dried over magnesium sulfate and concentrated on a rotary evaporator to a viscous oil residue, 133.2 g. Trituration of the residue with hexane gave a solid which was recrystallized from cold hexane to yield 52 g (62%) of white crystals, m.p. 72.5°-74° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05068231 |
| 出典データセット | uspto-grants-1991_11 |
| ORD ID | ord-af588826d4cf4c0aaa532385c2c04d5a |
| 出典メモ | uspto-grants-1991_11 |