Lithium Hydroxide → HCID 68808089, compound

HRID 1353039Notes

Reaction equation

HRID 1353039 reaction equation
[Li+].[OH-].[NH2:3][C:4]1[CH:5]=[C:6]([CH:27]=[CH:28][CH:29]=1)[C:7]([NH:9][CH2:10][C:11]([NH:13][CH:14]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:15][C:16]([O:18]CC)=[O:17])=[O:12])=[O:8].[F:30][C:31]([F:36])([F:35])[C:32]([OH:34])=[O:33]>O.C(O)C>[F:30][C:31]([F:36])([F:35])[C:32]([OH:34])=[O:33].[NH2:3][C:4]1[CH:5]=[C:6]([CH:27]=[CH:28][CH:29]=1)[C:7]([NH:9][CH2:10][C:11]([NH:13][CH:14]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[CH2:15][C:16]([OH:18])=[O:17])=[O:12])=[O:8]

Participants

6

Reactant 3

HCID 3939Lithium HydroxideHCID 6422Trifluoroacetic acidHCID 21101496HCID 21101496, compound

Product 1

HCID 68808089HCID 68808089, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

LiOH x H2O (648 mg) was added to a solution of ethyl 3-{2-[(3-(amino)-benzoyl)amino]acetamido}-3-phenyl-propanoate from II.3b (1.5 g) in 300 ml of water and the mixture was stirred at room temperature for 24 h. It was then neutralized with trifluoroacetic acid and concentrated. After chromatographic purification (methylene chloride/methanol (2:1)), a solid was isolated. This was taken up in ethanol, filtered and a white solid was obtained after concentration of the filtrate (yield: 1.4 g).

Workup

  1. concentrationconcentrated
  2. customAfter chromatographic purification (methylene chloride/methanol (2:1))
  3. customa solid was isolated
  4. filtrationfiltered

Sources & evidence

ORD record
ord-eed9335f85684717ba56765f29d209f4
Source dataset
uspto-grants-2007_05
Patent number
US07220824B1

Reaction notes

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