関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chlorobenzoxazole | HCID 11986 | — |
| 反応物 | 2,9-Diazaspiro(5.5)undecan-1-one hydrochloride | HCID 45074288 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 9-(Benzo[d]oxazol-2-yl)-2,9-diazaspiro[5.5]undecan-1-one | HCID 67253712 | 72% |
反応手順
To the stirred solution of 2,9-diazaspiro[5.5]undecan-1-one hydrochloride [1187173-73-4] (100 mg, 0.49 mmol) in DMF (3 mL) was added K2CO3 (203 mg, 1.47 mmol) and 2-chloro benzoxazole [615-18-9] (82.8 mg, 0.54 mmol). The mixture was heated at 60° C. for 18 h. The reaction mixture was cooled to rt and concentrated under reduced pressure. To the crude mixture water was added and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated to obtain a yellow solid which was washed with diethyl ether and n-pentane to yield the title compound as solid (100 mg, 72%). [LCMS RtF=0.36 min, [M+H]+=286.1]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530648B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-7d8c0276c0d2440aabcc1643f268cfba |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|