Hydrochloric Acid → HCID 129712714, compound

HRID 1383759Notes

Reaction equation

HRID 1383759 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

4

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

  1. customThe water is eliminated on a rotary evaporator under reduced pressure
  2. customAfter evaporation, 1.1 g of a pale yellow solid
  3. customare obtained
  4. 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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