Lithium hydroxide, monohydrate → HCID 69655912, compound

HRID 11699Notes

Reaction equation

HRID 11699 reaction equation
C([O:3][C:4](=[O:35])[CH:5]([NH2:34])[CH2:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[O:14][CH2:15][C:16]([N:18]1[CH2:23][C@H:22]([CH3:24])[N:21]([CH2:25][C:26]2[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=2)[CH2:20][C@H:19]1[CH3:33])=[O:17])C.O.[OH-].[Li+]>O1CCCC1.CO.O>[NH2:34][CH:5]([CH2:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[O:14][CH2:15][C:16]([N:18]1[CH2:23][C@H:22]([CH3:24])[N:21]([CH2:25][C:26]2[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=2)[CH2:20][C@H:19]1[CH3:33])=[O:17])[C:4]([OH:35])=[O:3]

Participants

6

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 696554352-Amino-3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-propionic Acid Ethyl Ester

Product 1

HCID 69655912HCID 69655912, compound

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 2-amino-3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-propionic acid ethyl ester (0.033 g, 0.065 mmol) in tetrahydrofuran, methanol and water (1 ml each) was added lithium hydroxide hydrate (0.014 g, 0.33 mmol). After 3 hours the reaction was concentrated in vacuo and the title compound was isolated by chromatography on silica gel (0.031 g, LRMS 478.5).

Workup

  1. concentrationAfter 3 hours the reaction was concentrated in vacuo

Sources & evidence

ORD record
ord-176e1dc368da4bdc88c934844ede6c9f
Source dataset
uspto-grants-2006_08
Patent number
US07098212B2

Reaction notes

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