Lithium hydroxide, monohydrate → HCID 21963704, compound

HRID 2212183Notes

Reaction equation

HRID 2212183 reaction equation
O.[OH-].[Li+].C([O:6][C:7](=[O:31])[CH2:8][N:9]1[CH2:14][CH2:13][CH2:12][CH:11]([N:15]2[C:24]3[CH:23]=[CH:22][CH:21]=[C:20]([Cl:25])[C:19]=3[C:18]3=[N:26][O:27][C:28]([CH3:29])=[C:17]3[C:16]2=[O:30])[CH2:10]1)C>O.O1CCOCC1.C(Cl)(Cl)Cl>[Cl:25][C:20]1[C:19]2[C:18]3[C:17](=[C:28]([CH3:29])[O:27][N:26]=3)[C:16](=[O:30])[N:15]([CH:11]3[CH2:12][CH2:13][CH2:14][N:9]([CH2:8][C:7]([OH:31])=[O:6])[CH2:10]3)[C:24]=2[CH:23]=[CH:22][CH:21]=1

Participants

6

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 69652382HCID 69652382, compound

Product 1

HCID 21963704HCID 21963704, compoundYield 122.2%

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 6212ChloroformSolventHCID 312751,4-DioxaneSolvent

Procedure

Add a solution of lithium hydroxide monohydrate (7 mg, 0.17 mmol) in water (2 mL) to a solution of [3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidin-1-yl]-acetic acid ethyl ester (45.7 mg, 0.11 mmol) in dioxane (3 mL). Stir the reaction at room temperature for 1 hour. Concentrate the reaction. Dissolve in chloroform and concentrate (×3) to assist in removal of solvents to yield the resulting 50.5 mg of the title compound as a white solid, quantitative yield. MS (ion spray) 376 (M+).

Workup

  1. customthe reaction at room temperature for 1 hour
  2. concentrationConcentrate
  3. customthe reaction
  4. concentrationconcentrate (×3)
  5. customto assist in removal of solvents

Sources & evidence

ORD record
ord-b71864b764304f478f66bf4e43c733c1
Source dataset
uspto-grants-2006_09
Patent number
US07101891B2

Reaction notes

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