関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Perfluoro-1-butanesulfonyl fluoride | HCID 67814 | — |
| 反応物 | Methyl 2-hydroxy-1-naphthoate | HCID 598533 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-(perfluoro-1-butanesulfonyloxy)-1-napthoate | HCID 18353806 | — |
反応手順
Perfluoro-1-butanesulfonyl fluoride (19 mL, 106 mmol, 1 eq) was added to a solution of methyl 2-hydroxy-1-naphthoate (21.25 g, 105 mmol, 1 eq) and triethylamine (15 mL, 108 mmol, 1 eq) in tetrahydrofuran (150 mL) maintained at an internal temperature about 0° C., under nitrogen. Once the addition was complete, the mixture was allowed to warm to ambient temperature and stirred for 64 hours. Toluene (150 mL) was added causing some precipitation. The solids were removed by filtration through Celiteä and washed with toluene (20 mL). The organic solutions were combined and washed with 2 N HCl (aq) (2×50 mL), water (100 mL), saturated aqueous sodium carbonate solution (100 mL) and brine (100 mL). The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure. Yield 48.79 g, 95%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06320068B1 |
|---|
| 出典データセット | uspto-grants-2001_11 |
|---|
| ORD ID | ord-0b6ac454dd9f4f31a52a4a5d6e0de927 |
|---|
| 出典メモ | uspto-grants-2001_11 |
|---|