HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butanol → 2-(Boc-amino)-4-methylthiophene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | 4-Methylthiophene-2-carboxylic acid | HCID 2794584 | — |
| Product | 2-(Boc-amino)-4-methylthiophene | HCID 57471983 | — |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318755B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-435b81a347a74151b4ac8092efbc7b8e |
| Source note | uspto-grants-2012_11 |