Lithium Hydroxide → HCID 68154501, compound

HRID 1615757Notes

Reaction equation

HRID 1615757 reaction equation
[OH-].[Li+].[F:3][C:4]1[CH:5]=[C:6]([CH:10]2[N:15]([CH2:16][C:17]([O:19]C)=[O:18])[C:14](=[O:21])[C:13]3([CH2:27][O:26][CH2:25][CH2:24][O:23][CH2:22]3)[N:12]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:11]2)[CH:7]=[CH:8][CH:9]=1>C1COCC1.O>[C:31]([O:30][C:28]([N:12]1[C:13]2([CH2:27][O:26][CH2:25][CH2:24][O:23][CH2:22]2)[C:14](=[O:21])[N:15]([CH2:16][C:17]([OH:19])=[O:18])[CH:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([F:3])[CH:5]=2)[CH2:11]1)=[O:29])([CH3:34])([CH3:32])[CH3:33]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 68154152HCID 68154152, compound

Product 1

HCID 68154501HCID 68154501, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

15 mg (0.62 mmol) lithium hydroxide were added to 0.25 g (0.55 mmol) tert-butyl 3-(3-fluorophenyl)-4-(2-methoxy-2-oxoethyl)-5-oxo-8,11-dioxa-1,4-diazaspiro[5.6]dodecane-1-carboxylate in 5 ml THF and 1 ml of water. The mixture was stirred for 2 h at RT and then the MeOH was distilled off. The residue was mixed with water and acidified with formic acid. The aqueous phase was extracted with ethyl acetate. The ethyl acetate phase was dried and evaporated down.

Workup

  1. distillationthe MeOH was distilled off
  2. additionThe residue was mixed with water
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialThe ethyl acetate phase was dried
  5. customevaporated down

Sources & evidence

ORD record
ord-10be0c07c94943f289ba4bf86d9736c9
Source dataset
uspto-grants-2014_07
Patent number
US08765763B2

Reaction notes

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