Lithium hydroxide, monohydrate → HCID 18542421, compound

HRID 1267933Notes

Reaction equation

HRID 1267933 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([NH:13][C:14]2[C:15]([CH3:24])=[C:16]([CH:21]=[CH:22][CH:23]=2)[C:17]([O:19]C)=[O:18])=[O:12])[CH:5]=[CH:6][C:7]=1[F:8].O.[OH-].[Li+]>CO.O>[F:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([NH:13][C:14]2[C:15]([CH3:24])=[C:16]([CH:21]=[CH:22][CH:23]=2)[C:17]([OH:19])=[O:18])=[O:12])[CH:5]=[CH:6][C:7]=1[F:8]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 86758938HCID 86758938, compound

Product 1

HCID 18542421HCID 18542421, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A mixture of the product from step (c) (1.33 g) and lithium hydroxide monohydrate (0.84 g) in methanol (120 ml) and water (25 ml) was heated at reflux for 2 hours, cooled and concentrated in vacuo. The residual aqueous solution was acidified with glacial acetic acid and extracted with ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4) and evaporated to give a cream solid. Yield 1.27 g.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperaturecooled
  4. concentrationconcentrated in vacuo
  5. extractionextracted with ethyl acetate
  6. washThe combined extracts were washed with water and brine
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customto give a cream solid

Sources & evidence

ORD record
ord-6faa66adfc6041ac8567d6b70a68915a
Source dataset
uspto-grants-2003_04
Patent number
US06555541B1

Reaction notes

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