Lithium hydroxide, monohydrate → HCID 19378943, compound

HRID 2210576Notes

Reaction equation

HRID 2210576 reaction equation
O.[OH-].[Li+].[C:4]([O:8][C:9]([N:11]([CH2:13][C:14]1[N:15]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[C:40]([C:42]([O:44]C)=[O:43])=[O:41])=[CH:30][CH:29]=2)[C:16]([C:23]([O:25]C)=[O:24])=[C:17]([C:19]([OH:22])([CH3:21])[CH3:20])[N:18]=1)[CH3:12])=[O:10])([CH3:7])([CH3:6])[CH3:5]>O.O1CCOCC1>[C:4]([O:8][C:9]([N:11]([CH2:13][C:14]1[N:15]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[C:40]([C:42]([OH:44])=[O:43])=[O:41])=[CH:30][CH:29]=2)[C:16]([C:23]([OH:25])=[O:24])=[C:17]([C:19]([OH:22])([CH3:21])[CH3:20])[N:18]=1)[CH3:12])=[O:10])([CH3:5])([CH3:6])[CH3:7]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 19378958HCID 19378958, compound

Product 1

HCID 19378943HCID 19378943, compoundYield 93.7%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

A solution of 81 mg of lithium hydroxide monohydrate dissolved in 5 ml of water was added to a solution of 380 mg of methyl 2-(N-t-butoxycarbonyl-N-methylaminomethyl)-4-(1-hydroxy-1-methylethyl)-1-[(2'-methoxalylbiphenyl-4-yl)methyl]imidazole-5-carboxylate [prepared as described in step (a) above] dissolved in 5 mg of dioxane, and the resulting mixture was stirred at room temperature for 2.5 hours. At the end of this time, the dioxane was removed by distillation under reduced pressure, and then 1.93 ml of 1N aqueous hydrochloric acid was added to the residue. The material which precipitated was collected by filtration to give 339 mg of the title compound as an amorphous powder.

Workup

  1. customAt the end of this time, the dioxane was removed by distillation under reduced pressure
  2. addition1.93 ml of 1N aqueous hydrochloric acid was added to the residue
  3. customThe material which precipitated
  4. filtrationwas collected by filtration

Sources & evidence

ORD record
ord-bcad4a0bb1ae41c39917ea270afd1c67
Source dataset
uspto-grants-1995_10
Patent number
US05459148

Reaction notes

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