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tert-Butanol → 2-(Boc-amino)-4-methylthiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | 4-Methylthiophene-2-carboxylic acid | HCID 2794584 | — |
| 生成物 | 2-(Boc-amino)-4-methylthiophene | HCID 57471983 | — |
反応手順
A solution of 4-methyl thiophene-2-carboxylic acid (1.42 g, 10.0 mmol), triethylamine (1.50 mL, 10.8 mmol) and diphenyl phosphoryl azide (2.15 mL, 10.0 mmol) in tBuOH (20 mL) was stirred at reflux for 5 h. tBuOH was removed in vacuo. Et2O and water were added. The organic phase was washed with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, which was eluted with 0-10% EtOAc in hexane to give tert-butyl 4-methylthiophen-2-ylcarbamate as a solid (0.880 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08349860B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-b6a1908829e94859ab0233b71b884e78 |
| 出典メモ | uspto-grants-2013_01 |