Hydrochloric Acid → HCID 70237561, compound

HRID 370288Notes

Reaction equation

HRID 370288 reaction equation
[C:1]([CH2:4][O:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]1)(=[O:3])N.[ClH:21].[OH2:22]>>[ClH:21].[ClH:21].[N:8]1([CH2:7][CH2:6][O:5][CH2:4][C:1]([OH:3])=[O:22])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 21188361HCID 21188361, compound

Product 1

HCID 70237561HCID 70237561, compoundYield 88%

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 Buchi 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)ethoxyacetic acid dihydrochloride are obtained in the form of white crystals.

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-fd5a186b7c1441eea6ebe55c0f1e3b67
Source dataset
uspto-grants-2000_10
Patent number
US06140501

Reaction notes

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