Hydrochloric Acid → HCID 18381652, compound

HRID 2297502Notes

Reaction equation

HRID 2297502 reaction equation
[CH3:1][O:2][C:3]1[C:4]([C:14]#[C:15][Si](C)(C)C)=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[NH:8][N:7]=[CH:6]2.[OH-].[Na+].Cl>C(#N)C>[C:14]([C:4]1[C:3]([O:2][CH3:1])=[CH:12][CH:11]=[C:10]2[C:5]=1[CH:6]=[N:7][NH:8][C:9]2=[O:13])#[CH:15]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18381612HCID 18381612, compound

Product 1

HCID 18381652HCID 18381652, compoundYield 97.5%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A suspension of 6-methoxy-5-trimethylsilanylethynyl-2H-phthalazin-1-one (2.87 g, 10.20 mmoles), prepared as described in example 139, in acetonitrile (50 ml) was added with 32% NaOH (15 ml) and stirred at room temperature for 1 hour. The mixture was neutralised with concentrated HCl and the precipitate filtered off. The aqueous phase was extracted with ethyl acetate, the organic phase was dried and taken up in acetone. The solid was filtered off and joined to the previous precipitate to give 1.99 g of the title compound (yield: 97.3%).

Workup

  1. customprepared
  2. filtrationthe precipitate filtered off
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. customthe organic phase was dried
  5. filtrationThe solid was filtered off

Sources & evidence

ORD record
ord-7f4979c4ae9b462f8c3029a3c5dafac4
Source dataset
uspto-grants-2002_12
Patent number
US06492360B1

Reaction notes

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