関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 反応物 | 6-Hydroxy-3,4-dihydro-1(2H)-naphthalenone | HCID 4679494 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Oxo-5,6,7,8-tetrahydronaphthalen-2-yl trifluoromethanesulfonate | HCID 11098384 | — |
反応手順
Trifluoro-methanesulfonic anhydride (14.35 mL, 77.3 mmol) was added to a CH2Cl2 (150 mL) solution of 6-hydroxy-3,4-dihydro-2H-naphthalen-1-one (11.40 g, 70.3 mmol), N-methylmorpholine (8.5 mL, 77.3 mmol) and DMAP (130 mg, 1 mmol) in 5 min at −80° C. The mixture was warmed to 0° C. in 1 h then poured into a cold solution of saturated NH4Cl. The mixture was diluted with CH2Cl2 (400 mL), washed with H2O, dried over MgSO4, filtered, and concentrated in vacuo to provide the crude compound which was purified by column chromatography (silica, 0 to 60% CH2Cl2 in hexane) to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07425631B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-3b582824b37743d5aefae7d5d204232e |
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| 出典メモ | uspto-grants-2008_09 |
|---|
