Water → HCID 131714311, compound

HRID 280791Notes

Reaction equation

HRID 280791 reaction equation
[CH2:1]([P:8]([NH:17][C@H:18]([C:20]([N:22]1[CH2:36][CH2:35][CH2:34][C@H:23]1[C:24]([N:26]1[CH2:33][CH2:32][CH2:31][C@H:27]1[C:28]([OH:30])=[O:29])=[O:25])=[O:21])[CH3:19])([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[O-2].[Ca+2:39]>C(OCC)(=O)C>[Ca+2:39].[CH2:1]([P:8]([NH:17][C@H:18]([C:20]([N:22]1[CH2:36][CH2:35][CH2:34][C@H:23]1[C:24]([N:26]1[CH2:33][CH2:32][CH2:31][C@H:27]1[C:28]([O-:30])=[O:29])=[O:25])=[O:21])[CH3:19])([CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:1]([P:8]([NH:17][C@H:18]([C:20]([N:22]1[CH2:36][CH2:35][CH2:34][C@H:23]1[C:24]([N:26]1[CH2:33][CH2:32][CH2:31][C@H:27]1[C:28]([O-:30])=[O:29])=[O:25])=[O:21])[CH3:19])([CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 962WaterHCID 6850728CalciumoxideHCID 13503349HCID 13503349, compound

Product 1

HCID 131714311HCID 131714311, compoundYield 83.8%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Dibenzylphosphoryl-L-alanyl-L-prolyl-L-proline (0.5 g, 0.9 mmole) was dissolved in ethyl acetate (15 ml) which had been previously saturated with water, and calcium oxide (50, 0.9 mmol) was added thereto. The mixture was stirred for 2 hours at room temperature. Excess of calcium oxide was removed by filtration, and from the filtrate the solvent was distilled off under reduced pressure. The thus obtained residue was dissovled in ethyl acetate, and n-hexane was added thereto while stirring to obtain dibenzylphosphoryl-L-alanyl-L-prolyl-L-proline calcium salt (0.40 g).

Workup

  1. additionwas added
  2. customExcess of calcium oxide was removed by filtration
  3. distillationfrom the filtrate the solvent was distilled off under reduced pressure
  4. additionn-hexane was added
  5. stirringwhile stirring

Sources & evidence

ORD record
ord-cecb99b327504db0b8c305aa4a0e95ea
Source dataset
uspto-grants-1986_05
Patent number
US04590178

Reaction notes

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