Lithium Hydroxide → HCID 22097163, compound

HRID 1458860Notes

Reaction equation

HRID 1458860 reaction equation
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([NH:6][C:7](=[O:18])[C:8](=[O:17])[N:9]2[CH2:12][C:13]([O:15]C)=[O:14])=[CH:4][C:3]=1[N:19]1[C:23]([CH3:24])=[CH:22][CH:21]=[C:20]1[CH3:25].[OH-].[Li+]>O1CCCC1.O>[C:13]([CH2:12][N:9]1[C:10]2[C:5](=[CH:4][C:3]([N:19]3[C:23]([CH3:24])=[CH:22][CH:21]=[C:20]3[CH3:25])=[C:2]([Cl:1])[CH:11]=2)[NH:6][C:7](=[O:18])[C:8]1=[O:17])([OH:15])=[O:14]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 22097066HCID 22097066, compound

Product 1

HCID 22097163HCID 22097163, compoundYield 84.1%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

4.0 g (10.6 mmol) of 7-chloro-6-(2,5-dimethyl-1-pyrrolyl)-1-(methoxycarbonylmethyl)-2,3(1H,4H)-quinoxalinedione (Example 44) were dissolved in 100 ml of tetrahydrofuran, and a solution of 0.76 g (31.9 mmol) of lithium hydroxide in 15 ml of water was added. The mixture was stirred at room temperature for 2 h and then the organic solvent was removed under reduced pressure, and the aqueous phase was acidified with 1M hydrochloric acid. The precipitate was filtered off with suction to yield 3.1 g (84%) of the product. Melting point >265° C.

Workup

  1. customthe organic solvent was removed under reduced pressure
  2. filtrationThe precipitate was filtered off with suction

Sources & evidence

ORD record
ord-b9bd112ec3d6412ab3f917055d93413c
Source dataset
uspto-grants-1998_12
Patent number
US05852017

Reaction notes

Loading…