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Diethylamine → 3-benzyloxy-N,N-diethyl-4-methoxy-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | 3-Benzyloxy-4-methoxybenzoyl chloride | HCID 10967795 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-benzyloxy-N,N-diethyl-4-methoxy-benzamide | HCID 18504804 | 91% |
反応手順
A solution of diethylamine (548 ml, 5.3 moles) in CH2Cl2 (452 ml) was added dropwise to a solution of 3-benzyloxy-4-methoxy-benzoyl chloride (146.66 g, 0.53 moles), obtained as described in example 30, in methylene chloride (640 ml), at 0° C. under nitrogen, at constant temperature. At the end the temperature was left to arise to the room value. After 2 hours the mixture was evaporated, taken up with ethyl acetate and washed with water. The organic phase was dried and concentrated to give a solid which, triturated twice with heptane and once with petrolatum, then dried at 45° C. under vacuum gave 150.62 g of the title compound (yield: 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06340684B1 |
| 出典データセット | uspto-grants-2002_01 |
| ORD ID | ord-d18cfc26bba84e66a2d0e0bc4972c7c4 |
| 出典メモ | uspto-grants-2002_01 |