Lithium Hydroxide → HCID 117874295, compound

HRID 2272864Notes

Reaction equation

HRID 2272864 reaction equation
[CH:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH:4]1[C:16]([O:18]C)=[O:17])=[O:2].[Li+:20].[OH-]>O1CCOCC1.O>[C:12]([O:11][C:9]([N:6]1[CH2:7][CH2:8][N:3]([CH:1]=[O:2])[CH:4]([C:16]([O-:18])=[O:17])[CH2:5]1)=[O:10])([CH3:15])([CH3:13])[CH3:14].[Li+:20]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 59437100HCID 59437100, compound

Product 1

HCID 117874295HCID 117874295, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

To a solution of 28 g of the compound obtained in Step A (103 mmol) in 515 mL of dioxane there are added 4.8 g of LiOH (113 mmol) in solution in 100 mL of H2O. The whole is stirred at ambient temperature for 4 hours. The reaction mixture is subsequently concentrated to dryness and then co-evaporated several times with ethyl acetate. The title product is obtained in the form of a solid and is used directly for the following cyclisation step.

Workup

  1. concentrationThe reaction mixture is subsequently concentrated to dryness

Sources & evidence

ORD record
ord-90a616bd8469431999dff72bf40efa4b
Source dataset
uspto-grants-2015_09
Patent number
US09120791B2

Reaction notes

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