Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 21188359 | HCID 21188359 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21188365 | HCID 21188365 | 93% |
Reaction Steps
2 g (0.0066 mol) of tert-butyl 4-(2-methoxycarbonylmethoxyethyl)piperazine-1-carboxylate prepared in Example I.4.3. are dissolved in 5 ml of ethyl acetate in a 50 ml three-necked round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. 20 ml of a 3M solution of hydrochloric acid in ethyl acetate are added in a single portion with stirring. The mixture is stirred at room temperature for 30 minutes. 5 ml of a 3M solution of hydrochloric acid in ethyl acetate are then added and stirring is continued for 30 minutes. The precipitate is filtered off and is washed with 2×5 ml of ethyl acetate. 1.68 g (93%) of methyl 2-(1-piperazinyl)ethoxyacetate dihydrochloride are obtained in the form of a beige-colored solid. NMR: δ: 3.4 (2H, t, 4.8 Hz), 3.47-3.65 (8H, m); 3.67 (3H, s); 3.92 (2H, t, 4.8 Hz); 4.21 (2H, s); 10.1 (2H, bs). Mass spectrum: 202 (M+·).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06255487B1 |
|---|
| Source dataset | uspto-grants-2001_07 |
|---|
| ORD ID | ord-7b42da98155c4e72b913dc554a180ee7 |
|---|
| Source note | uspto-grants-2001_07 |
|---|