Lithium Hydroxide → HCID 57635120, compound

HRID 535973Notes

Reaction equation

HRID 535973 reaction equation
[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][N:5]2[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[N:10][C:11]([C:12]([O:14]CC)=[O:13])=[C:4]2[CH2:3]1.[OH-].[Li+]>CO.O>[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][N:5]2[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[N:10][C:11]([C:12]([OH:14])=[O:13])=[C:4]2[CH2:3]1

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 57635641HCID 57635641, compound

Product 1

HCID 57635120HCID 57635120, compoundYield 72.2%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Conditions

Temperature
50 °C

Procedure

To a solution of intermediate 64B (0.87 g, 2.91 mmol) in 20 mL methanol was added lithium hydroxide (0.139 g, 5.81 mmol) in 5 mL water. The reaction mixture was stirred at 50° C. for 2 hours, filtered, concentrated and neutralized with 1N HCl. The resulting solution was lyophilized to provide intermediate 64C (0.57 g, 72%) as a white solid. LCMS (+ESI) m/z 272.1 [M+H]+

Workup

  1. filtrationfiltered
  2. concentrationconcentrated

Sources & evidence

ORD record
ord-8c4d509ad04a4baf80d055f6dea803cd
Source dataset
uspto-grants-2014_10
Patent number
US08859538B2

Reaction notes

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