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1-Octanol → Octyl4'-methoxycarbonyloxy-4-biphenylcarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Octanol | HCID 957 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | 4'-Methoxycarbonyloxy-4-biphenylcarboxylic acid | HCID 18328408 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Octyl4'-methoxycarbonyloxy-4-biphenylcarboxylate | HCID 18328376 | — |
反応手順
A solution of triphenylphosphine (3.78 g, 0.014 mol) in dry tetrahydrofuran (50 ml) was added to a stirred solution of compound 4 (3.92 g, 0.014 mol), octan-1-ol (1.88 g 0.014 mol) and diethyl azodicarboxylate (DEAD) (2.51 g 0.014 mol) in dry tetrahydrofuran (100 ml) under an atmosphere of dry nitrogen. The addition was such that the triphenylphosphine was added over 30 seconds in which time the solution became hot and the white solid (4) and orange colour (DEAD) disappeared. The resultant solution was stirred overnight, the solvent was removed in vacuo and the viscous, oily residue was purified by column chromatography (10% petrol/dichloromethane) to give a colourless solid which was recrystallised from ethanol to leave colourless plates.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06278028B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-21b90c025f3a4e54907e42cc3e272c2f |
| 出典メモ | uspto-grants-2001_08 |