Hydrochloric Acid → HCID 129712714, compound
Reaction equation
[C:1]([CH2:4][O:5][CH2:6][CH2:7]N1CCN(C(OC(C)(C)C)=O)CC1)(=[O:3])N.[ClH:21].[OH2:22]>>[ClH:21].[ClH:21].[CH2:6]([O:5][CH2:4][C:1]([OH:3])=[O:22])[CH3:7]Participants
Conditions
- Temperature
- 60 °C
Procedure
1 g (0.00348 mol) of tert-butyl 4-(2-carbamoylmethoxyethyl)piperazine-1-carboxylate prepared in Example I.4.3. and 2 ml of water are placed in a 10 ml conical flask. 2 ml of 37% hydrochloric acid solution are added and the mixture is heated on an oil bath at 60° C. for 1 hour. The water is eliminated on a rotary evaporator under reduced pressure. The residue is taken up in toluene. After evaporation, 1.1 g of a pale yellow solid are obtained. This finely ground solid is placed in a Büchi sublimator. The apparatus is placed under vacuum (0.3 mmHg) and heated at 150° C. for 8 hours. 800 mg (88%) of 2-1-piperazinyl)ethoxy acetic acid dihydrochloride are obtained in the form of white crystals. The analyses correspond to those obtained with the compound prepared in Example I.1.4.
Workup
- customThe water is eliminated on a rotary evaporator under reduced pressure
- customAfter evaporation, 1.1 g of a pale yellow solid
- customare obtained
- temperatureheated at 150° C. for 8 hours
Sources & evidence
- ORD record
- ord-f881bad9f33440249f4f7fb04ea81c4f
- Source dataset
- uspto-grants-2001_07
- Patent number
- US06255487B1
Reaction notes
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