HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrofluoric Acid → Ethyl 4-methyl-1H-1,2,3-triazole-1-acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrofluoric Acid | HCID 14917 | — |
| Reactant | Ethyl 4-methyl-5-(trimethylsilyl)-1H-1,2,3-triazole-1-acetate | HCID 66839489 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 4-methyl-1H-1,2,3-triazole-1-acetate | HCID 59603650 | 94.2% |
Reaction Steps
To a solution of 0.77 g (3.2 mmol) of ethyl [4-methyl-5-(trimethylsilyl)-1H-1,2,3-triazole-1-yl]acetate from step A above in 2 mL of THF was added 1.3 mL (32 mmol) of a solution of 50% hydrofluoric acid in water. The resulting mixture was stirred at room temperature for 3 h and then evaporated to dryness in vacuo. Next, 5 mL of a 2.0 N ammonia in methanol solution was added and then the mixture was again evaporated to dryness in vacuo. The mixture was dissolved in dichloromethane, filtered and then evaporated in vacuo to afford the title compound as a clear gum (0.51 g. 93%). 1HNMR (500 MHz, CDCl3) δ: 7.5 (s, 1H), 5.05 (s, 2H), 4.23 (m, 2H), 2.30 (s, 3H), 1.30 (m, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653260B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-82eeffaef6cd4d59a6a15cec5d0a2eb3 |
| Source note | uspto-grants-2014_02 |