HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 4-Ethynyl4-hydroxy-tetrahydro-pyran-2-carboxylic Acid Amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 4-Hydroxy-4-trimethylsilanylethynyl-tetrahydro-pyran-2-carboxylic Acid Ethyl Ester | HCID 53667156 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-Ethynyl4-hydroxy-tetrahydro-pyran-2-carboxylic Acid Amide | HCID 53634009 | 97% |
Reaction Steps
4-Hydroxy-4-trimethylsilanylethynyl-tetrahydro-pyran-2-carboxylic acid ethyl ester (2.50 g, 9.25 mmol) was dissolved in MeOH (20 mL) in a pressure reaction tube and NH3 gas was passed through the solution for 10 minutes with stirring. The tube was tightly capped and the reaction was stirred for 3 days. After solvent removal, 1.53 g (97%) of yellow oil was obtained: 1H NMR (CD3OD) δ 1.48 (t, 1H), 1.70 (td, 1H), 1.85 (d, 1H), 2.30 (d, 1H), 3.04 (s, 1H), 3.29 (s, 1H), 3.71(t, 1H), 3.98 (d, 1H), 4.06 (dt, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06284764B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-9ee595eee8bf4a50ad95f3897ee32ce3 |
| Source note | uspto-grants-2001_09 |