Sulfuric Acid → HCID 70457844, compound

HRID 64787

Reaction equation

HRID 64787 reaction equation
[NH2:1][CH:2]([C:6]([OH:8])=[O:7])[CH:3]([CH3:5])[CH3:4].[C:9]([NH:19][C@H:20]([C:25]([OH:27])=[O:26])[CH2:21][C:22]([OH:24])=[O:23])([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10].S(=O)(=O)(O)O>O>[NH2:1][C@H:2]([C:6]([OH:8])=[O:7])[CH:3]([CH3:5])[CH3:4].[C:9]([NH:19][C@H:20]([C:25]([OH:27])=[O:26])[CH2:21][C:22]([OH:24])=[O:23])([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 1182DL-valineHCID 2723942N-(Benzyloxycarbonyl)aspartic acid

Product 1

HCID 70457844HCID 70457844, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
50 °C

Procedure

A 11.7 g portion of DL-valine, 13.4 g of N-carbobenzoxy-L-aspartic acid and 2.5 g of sulfuric acid were added to 50 ml of water and the resulting solution was heated to 50° C. This solution was cooled to 20° C. at a rate of 2° C. per hour while stirring, and was stirred for another two hours. The resulting crystal was separated, washed with 20 ml of water and dried to give 9.7 g of an L-valine/N-carbobenzoxy-L-aspartic acid salt. Analysis showed that the optical purity of the L-valine was 98%.

Workup

  1. temperatureThis solution was cooled to 20° C. at a rate of 2° C. per hour
  2. stirringwas stirred for another two hours
  3. customThe resulting crystal was separated
  4. washwashed with 20 ml of water
  5. customdried

Sources & evidence

ORD record
ord-8ac34c5e1fcf49c580b8b20a49cc16a8
Source dataset
uspto-grants-1986_09
Patent number
US04610827

Linked notes

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