Lithium hydroxide, monohydrate → HCID 9825896, compound

HRID 1069103Notes

Reaction equation

HRID 1069103 reaction equation
Cl.Cl.[CH3:3][O:4][C:5]([C:7]1[C:8]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([NH:23][CH2:24][CH2:25][NH:26][CH2:27][C@@H:28]([C:30]3[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=3)[OH:29])[CH:18]=2)=[CH:9][CH:10]=[C:11]([C:13]([O:15]C)=[O:14])[CH:12]=1)=[O:6].O.[OH-].[Li+]>CO.O>[OH-:4].[NH4+:23].[CH3:3][O:4][C:5]([C:7]1[C:8]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([NH:23][CH2:24][CH2:25][NH:26][CH2:27][C@@H:28]([C:30]3[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=3)[OH:29])[CH:18]=2)=[CH:9][CH:10]=[C:11]([C:13]([OH:15])=[O:14])[CH:12]=1)=[O:6]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 69780319HCID 69780319, compound

Product 2

HCID 14923Ammonium HydroxideHCID 9825896HCID 9825896, compoundYield 20.4%

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Procedure

The product was prepared from (R)-3′-[[2-[[2-(3-chlorophenyl)-2-hydroxyethyl]amino]ethyl]amino]-[1,1′-biphenyl]-2,4-dicarboxylic acid dimethyl ester dihydrochloride (406 mg) and lithium hydroxide monohydrate (262 mg) in 3:1 methanol-water (20 mL). Silica gel chromatography eluting with 6:2:0.1 chloroform:methanol:ammonium hydroxide afforded the title compound (35 mg) as a white solid.

Workup

  1. washSilica gel chromatography eluting with 6:2:0.1 chloroform

Sources & evidence

ORD record
ord-e15535e62ee04e0fb2639e5414680366
Source dataset
uspto-grants-2001_06
Patent number
US06251925B1

Reaction notes

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