関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | [2-(4-Trifluoromethyl-phenyl)-ethyl]-carbamic acid ethyl ester | HCID 66801630 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 7-(Trifluoromethyl)-3,4-dihydroisoquinolin-1(2H)-one | HCID 66801593 | 20.24% |
反応手順
Using the same procedure and workup as described in Example 1, step 4, [2-(4-trifluoromethyl-phenyl)-ethyl]-carbamic acid ethyl ester (I-16b: 2.7 g, 10.340 mmol) in POCl3 (15 mL) was reacted with P2O5 (2.92 g, 20.69 mmol). The resulting mixture was stirred at 105° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (2% methanol in DCM) afforded 450 mg of the product (20.24% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08946260B2 |
|---|
| 出典データセット | uspto-grants-2015_02 |
|---|
| ORD ID | ord-89bd677239e44ab5b799c78ce4d615ba |
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| 出典メモ | uspto-grants-2015_02 |
|---|
