Lithium Hydroxide → HCID 68872394, compound

HRID 1986400Notes

Reaction equation

HRID 1986400 reaction equation
[NH2:1][C:2]1[C:3]([C:7]2[N:8]([CH2:27][CH3:28])[C:9]3[CH:14]=[C:13]([CH2:15][C:16]4[CH:17]=[C:18]([CH:23]=[CH:24][CH:25]=4)[C:19]([O:21]C)=[O:20])[N:12]=[CH:11][C:10]=3[N:26]=2)=[N:4][O:5][N:6]=1.[Li+].[OH-]>CO.O>[NH2:1][C:2]1[C:3]([C:7]2[N:8]([CH2:27][CH3:28])[C:9]3[CH:14]=[C:13]([CH2:15][C:16]4[CH:17]=[C:18]([CH:23]=[CH:24][CH:25]=4)[C:19]([OH:21])=[O:20])[N:12]=[CH:11][C:10]=3[N:26]=2)=[N:4][O:5][N:6]=1

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 68875464HCID 68875464, compound

Product 1

HCID 68872394HCID 68872394, compoundYield 83.6%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Conditions

Temperature
80 °C

Procedure

To a solution of the product from Step 1 (85 mg, 0.22 mmol) in MeOH (12 ml) and water (4 ml), was added LiOH (40 mg, 0.95 mmol). This mixture was then heated to 80° C. for 2 h. Reaction mixture was concentrated, dissolved in 10 ml water, acidified with 1 N HCl to pH=5, then filtered and washed with water to afford a pale yellow solid (67 mg, 82%). MS (ES+) m/e 365 [M+H]+.

Workup

  1. customReaction mixture
  2. concentrationwas concentrated
  3. dissolutiondissolved in 10 ml water
  4. filtrationfiltered
  5. washwashed with water

Sources & evidence

ORD record
ord-0192ebb0a048457ab465b11ff2d7794b
Source dataset
uspto-grants-2009_06
Patent number
US07547779B2

Reaction notes

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