Lithium hydroxide, monohydrate → HCID 68700284, compound

HRID 1437383Notes

Reaction equation

HRID 1437383 reaction equation
C[O:2][C:3]([C@@H:5]1[CH2:10][CH2:9][C@@H:8]([NH:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[C@H:7]([O:19][CH3:20])[CH2:6]1)=[O:4].O.[OH-].[Li+]>CO.O>[C:15]([O:14][C:12]([NH:11][C@@H:8]1[CH2:9][CH2:10][C@@H:5]([C:3]([OH:4])=[O:2])[CH2:6][C@H:7]1[O:19][CH3:20])=[O:13])([CH3:18])([CH3:17])[CH3:16]

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 68695542HCID 68695542, compound

Product 1

HCID 68700284HCID 68700284, compoundYield 96.3%

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Procedure

The ester (e) (5.47 g, 19 mmol) and lithium hydroxide monohydrate (0.96 g, 23 mmol) in methanol/water (50 ml/50 ml) were stirred at room temperature for 18 hours then evaporated to dryness. The residue was partitioned between ethyl acetate and water (30 ml) containing sodium dihydrogen phosphate (7 g). The aqueous phase was further extracted with ethyl acetate and the combined extracts washed with brine, dried and evaporated to give a solid (5.0 g, 96%).

Workup

  1. customthen evaporated to dryness
  2. customThe residue was partitioned between ethyl acetate and water (30 ml)
  3. additioncontaining sodium dihydrogen phosphate (7 g)
  4. extractionThe aqueous phase was further extracted with ethyl acetate
  5. washthe combined extracts washed with brine
  6. customdried
  7. customevaporated

Sources & evidence

ORD record
ord-ef2fbc2a6f80418985aff49a83e64b0e
Source dataset
uspto-grants-2009_11
Patent number
US07622481B2

Reaction notes

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