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Citric Acid → BOC-L-proline L-glutamic acid dibenzyl ester

HRID 2235819
Notes
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Reaction equation

HRID 2235819 reaction equation
[C:1]([N:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.ClC(OCC)=O.[CH2:29]([O:36][C:37](=[O:52])[C@H:38]([CH2:40][CH2:41][C:42]([O:44][CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)=[O:43])[NH2:39])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>ClCCl.C(=O)(O)[O-].[Na+]>[C:1]([N:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[CH2:29]([O:36][C:37](=[O:52])[C@H:38]([CH2:40][CH2:41][C:42]([O:44][CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)=[O:43])[NH2:39])[C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 311Citric AcidHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 850831,2-Pyrrolidinedicarboxylic acid, 1-(1,1-dimethylethyl) ester, (2S)-HCID 3037947L-Glutamic acid dibenzyl ester

Product 1

HCID 86608919
BOC-L-proline L-glutamic acid dibenzyl ester
Yield 95%

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 516892Sodium BicarbonateSolvent

Conditions

Temperature
0 °C

Procedure

To a solution of BOC-proline (Anderson G W and McGregor A C: J. Amer. Chem. Soc.: 79, 6810, 1994) (10 mmol) in dichloromethane (50 ml), cooled to 0° C., was added triethylamine (1.39 ml, 10 mmol) and ethyl chloroformate (0.96 ml, 10 mmol). The resultant mixture was stirred at 0° C. for 30 minutes. A solution of dibenzyl-L-glutamate (10 mmol) was then added and the mixture stirred at 0° C. for 2 hours then warmed to room temperature and stirred overnight. The reaction mixture was washed with aqueous sodium bicarbonate and citric acid (2 mol 1-1) then dried (MgSO4) and concentrated at reduced pressure to give BOC-L-proline-L-glutamic acid dibenzyl ester (5.0 g, 95%).

Workup

  1. temperaturethen warmed to room temperature
  2. stirringstirred overnight
  3. dry with materialthen dried (MgSO4)
  4. concentrationconcentrated at reduced pressure

Sources & evidence

ORD record
ord-27c4927a2e6b4e8cace9257fe01202e1
Source dataset
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07714020B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes