Lithium Hydroxide → HCID 70928939, compound

HRID 1479949Notes

Reaction equation

HRID 1479949 reaction equation
C[O:2][C:3]([C:5]1[N:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([C:17]3[N:18]=[N:19][C:20]([C:25]4[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=4)=[C:21]([CH3:24])[C:22]=3[CH3:23])[CH2:13][C@H:12]2[CH3:35])=[N:9][CH:10]=1)=[O:4].[Li+].[OH-]>CO>[F:34][C:31]([F:32])([F:33])[C:28]1[CH:27]=[CH:26][C:25]([C:20]2[N:19]=[N:18][C:17]([N:14]3[CH2:15][CH2:16][N:11]([C:8]4[CH:7]=[N:6][C:5]([C:3]([OH:4])=[O:2])=[CH:10][N:9]=4)[C@H:12]([CH3:35])[CH2:13]3)=[C:22]([CH3:23])[C:21]=2[CH3:24])=[CH:30][CH:29]=1

Participants

4

Reactant 2

HCID 3939Lithium HydroxideHCID 70975738HCID 70975738, compound

Product 1

HCID 70928939HCID 70928939, compoundYield 99.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of example 7 (0.26 g, 0.53 mmol) and methanol (10 mL) is added 50% aqueous LiOH aqueous (10 mL). The mixture is stirred at room temperature overnight. Solvent is removed. The residue is dissolved in water and acidified with 3N HCl to pH about 7 and extracted with ethyl acetate. The ethyl acetate layer is concentrated to afford the title compound (0.25 g, 98%) as a yellow solid.

Workup

  1. customSolvent is removed
  2. dissolutionThe residue is dissolved in water
  3. extractionextracted with ethyl acetate
  4. concentrationThe ethyl acetate layer is concentrated

Sources & evidence

ORD record
ord-34f4e868a79240f88b5492d443054ddb
Source dataset
uspto-grants-2016_08
Patent number
US09409871B2

Reaction notes

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