Hydrochloric Acid → HCID 54236535, compound

HRID 1088193Notes

Reaction equation

HRID 1088193 reaction equation
N[C@H:2]([C:7]([OH:9])=[O:8])[C@H:3]([CH2:5][CH3:6])[CH3:4].NC(N)=O.[ClH:14]>[N+]([O-])(O)=O>[Cl:14][C@@H:2]([CH:3]([CH3:4])[CH2:5][CH3:6])[C:7]([OH:9])=[O:8]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 1176UreaHCID 6306L-Isoleucine

Product 1

HCID 54236535HCID 54236535, compound

Reagents, catalysts & solvents 1

HCID 944Nitric AcidSolvent

Conditions

Temperature
80 °C

Procedure

To 20 g (0.150 moles) of L-(+)-isoleucine and 2 g of urea, 60 mL concentrated HCl and 30 mL concentrated HNO3 are added at room temperature. The mixture is subsequently heated for 1 hour at 80° C. and then for 1 hour at 50° C. on a water bath (complete dissolution of the acid with heavy foaming). After cooling, the solution is extracted with ether several times, the ether extract is washed with water and dried over calcium chloride, the solvent is distilled off in a rotary evaporator and the residue is fractionated under vacuum.

Workup

  1. dissolutionfor 1 hour at 50° C. on a water bath (complete dissolution of the acid with heavy foaming)
  2. temperatureAfter cooling
  3. extractionthe solution is extracted with ether several times
  4. extractionthe ether extract
  5. washis washed with water
  6. dry with materialdried over calcium chloride
  7. distillationthe solvent is distilled off in a rotary evaporator

Sources & evidence

ORD record
ord-71863ba9f5d44adea69b42015cfd2290
Source dataset
uspto-grants-1990_10
Patent number
US04961876

Reaction notes

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