Lithium hydroxide, monohydrate → HCID 57843550, compound

HRID 734279Notes

Reaction equation

HRID 734279 reaction equation
C[O:2][C:3](=[O:27])[C:4]([C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=1)([CH3:18])[CH2:5][CH2:6][N:7]1[CH2:15][CH2:14][N:13]2[CH:9]([CH2:10][CH2:11][S:12]2(=[O:17])=[O:16])[CH2:8]1.O[Li].O>O.C1COCC1>[Cl:26][C:21]1[CH:20]=[C:19]([C:4]([CH3:18])([CH2:5][CH2:6][N:7]2[CH2:15][CH2:14][N:13]3[CH:9]([CH2:10][CH2:11][S:12]3(=[O:16])=[O:17])[CH2:8]2)[C:3]([OH:27])=[O:2])[CH:24]=[CH:23][C:22]=1[Cl:25]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 57843561HCID 57843561, compound

Product 1

HCID 57843550HCID 57843550, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A mixture of 1.16 g (2.6 mmol) 2-(3,4-dichloro-phenyl)-4-(1,1-dioxo-hexahydro-1λ6-thia-5,7a-diaza-inden-5-yl)-2-methyl-butyric acid methyl ester and 0.123 g (2.9 mmol) LiOH.H2O in 40 mL water and 40 mL THF was stirred at room temperature for 48 h. After evaporation of THF the pH was adjusted to pH=2 with 2N HCl aq., evaporated to dryness, taken up in acetonitrile and evaporated (3×), The residue was dried at 60° C. under high vacuum and used without further purification in the consecutive amide coupling step. MS(m/e): 421.0 (MH+).

Workup

  1. customAfter evaporation of THF the pH
  2. customevaporated to dryness
  3. customevaporated (3×)
  4. customThe residue was dried at 60° C. under high vacuum
  5. customused without further purification in the consecutive amide coupling step

Sources & evidence

ORD record
ord-673fa99f8bcd4a388bf07f8ee13d22d4
Source dataset
uspto-grants-2009_09
Patent number
US07592345B2

Reaction notes

Loading…