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Triphenylphosphine → methyl (R)-7-(4-fluorophenyl)-7-(2-hydroxy-3,4,6-trimethylphenyl)heptanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2,3,5-Trimethylphenol | HCID 12769 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 反応物 | methyl (S)-7-(4-fluorophenyl)-7-hydroxyheptanoate | HCID 10562892 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | methyl (R)-7-(4-fluorophenyl)-7-(2-hydroxy-3,4,6-trimethylphenyl)heptanoate | HCID 10714337 | 33.6% |
反応手順
To a solution of 2,3,5-trimethylphenol (0.80 g, 5.9 mmol), methyl (S)-7-(4-fluorophenyl)-7-hydroxyheptanoate (0.30 g, 1.2 mmol) and triphenylphosphine (0.46 g, 1.8 mmol) in 1,2-dichloroethane (20 ml) was added at 10° C. a solution of 95% DEAD (0.54 ml) in 1,2-dichloroethane (5 ml) taking 30 minutes. The mixture was stirred for one hour at the same temperature range, then the solvent was distilled off under reduced pressure. The residue was subjected to a silica gel column chromatography to give 0.15 g of methyl (R)-7-(4-fluorophenyl)-7-(2-hydroxy-3,4,6-trimethylphenyl)heptanoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420363 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-9323b5e843c14389855dc61cea00165b |
| 出典メモ | uspto-grants-1995_05 |