関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Tert-butyl 3-(methanesulfonyloxy)azetidine-1-carboxylate | HCID 10753243 | — |
| 反応物 | 4-(Cyclopropylmethoxy)phenol | HCID 13755495 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Cyclopropylmethoxy-phenoxy)-azetidine-1-carboxylic acid tert-butyl ester | HCID 86689008 | — |
反応手順
A mixture of 2.6 g (10.4 mmol) 3-methanesulfonyloxy-azetidine-1-carboxylic acid tert-butyl ester, 1.7 g (10.4 mmol) 4-cyclopropylmethoxy-phenol and 6.7 g (20.7 mmol) Cs2CO3 in 60 mL DMF is stirred for 12 h at 80° C. Water is added and the mixture is extracted with ethyl acetate (2×). The combined organic layers are washed with NaHCO3 solution and are dried over MgSO4. The solvent is evaporated and the residue is purified by column chromatography (silica gel; PE/ethyl acetate; gradient 9:1→8:2) to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530461B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-01104f221ee24fd5bf1ed83c68ae1a3b |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
