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Triethylamine → N-(2-Methyl-2-propenyl)-3-[4-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | 2-Methylallylamine | HCID 76141 | — |
| 反応物 | 3-[4-(Trifluoromethyl)phenoxy]azetidine oxalate | HCID 12812500 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-Methyl-2-propenyl)-3-[4-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide | HCID 15053426 | 58.9% |
反応手順
A stirred solution of 3.6 g (0.022 mole) of 1,1'-carbonyldiimidazole in 75 ml of methylene chloride under nitrogen was treated with 1.6 g (0.022 mole) of 2-methyl-2-propenylamine (added via a syringe and needle through a septum placed in one neck of the reaction flask). After stirring for 1 hr, 6.2 g (0.02 mole) of 3-[4-(trifluoromethyl)phenoxy]azetidine oxalate was added all at once followed in 30 min with 5 ml of triethylamine and stirring was continued for 3 hr. The reaction mixture was washed with water (2×25 ml), dried over magnesium sulfate and concentrated in vacuo. The oily residue solidified on standing and was recrystallized from isopropyl ether to yield 3.7 g (58.9%) of fine white crystals, m.p. 101°-102° 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-2c6dd84aad9f4a2e9b20996cd93451c3 |
| 出典メモ | uspto-grants-1991_11 |