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3,3-Dimethylcyclobutane-1,1-dicarboxylic acid → 3,3-Dimethylcyclobutanecarboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,3-Dimethylcyclobutane-1,1-dicarboxylic acid | HCID 14789766 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3,3-Dimethylcyclobutanecarboxylic acid | HCID 215106 | 91.3% |
反応手順
A solution of Intermediate 285C (250 mg, 1.452 mmol) in pyridine (5 mL) was stirred at 120° C. for 16 h. The reaction mixture was then cooled to RT, quenched with a 1.5 N aq. solution of HCl at 0° C., and extracted with diethyl ether (2×50 mL). The combined organic layers were washed with brine, dried over Na2SO4 and evaporated to afford Intermediate 285D as a viscous liquid (170 mg, 91% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.90-3.02 (m, 1H), 1.84-1.95 (m, 4H), 1.07-1.14 (m, 3H), 0.99-1.07 (m, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09273058B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-2d2d330610a44b41a30a78da0b5fd35d |
| 出典メモ | uspto-grants-2016_03 |