化工社化工社 化学情報印刷レポート · 研究参考用
2-(Trifluoromethyl)benzylic alcohol → 2-(Trifluoromethyl)benzyl 7-bromo-3-oxo-2,3-dihydrospiro[indene-1,4'-piperidine]-1'-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Trifluoromethyl)benzylic alcohol | HCID 67666 | — |
| 反応物 | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| 反応物 | 7-bromospiro[indene-1,4'-piperidin]-3(2H)-one | HCID 58295671 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Trifluoromethyl)benzyl 7-bromo-3-oxo-2,3-dihydrospiro[indene-1,4'-piperidine]-1'-carboxylate | HCID 44227079 | — |
反応手順
To o-(trifluoromethyl)benzyl alcohol (35 mg, 0.20 mmol) in CH2Cl2 (4 mL) was added was a solution of carbonyl diimidazole (29 mg, 0.18 mmol) in CH2Cl2 (4 mL). The mixture was stirred at rt for 2 h. A 1-mL aliquot of the resulting solution (0.05 mmol) was added to a solution 7-bromospiro[indene-1,4′-piperidin]-3(2H)-one (14.5 mg, 0.05 mmol) in CH2Cl2 (1 mL). The mixture was stirred at rt for 16 h, concentrated, redissolved in MeCN (1 mL) and heated at 60° C. for 2 h. Prep HPLC afforded the title compound. LC-MS Method 1 tR=2.06, min, m/z=484, 482.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383629B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-67ab8ad46ead4b3d99d43255073f14ae |
| 出典メモ | uspto-grants-2013_02 |