Water → HCID 23203297, compound

HRID 963191Notes

Reaction equation

HRID 963191 reaction equation
FC(F)(F)C(O)=O.[C:8]([N:12]1[C:17](=[O:18])[C:16]([CH:19]2OC(C)CC[O:20]2)=[C:15]([NH:26][CH2:27][C:28]2[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=2)[CH:14]=[N:13]1)([CH3:11])([CH3:10])[CH3:9].O>C(OCC)(=O)C>[C:8]([N:12]1[C:17](=[O:18])[C:16]([CH:19]=[O:20])=[C:15]([NH:26][CH2:27][C:28]2[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=2)[CH:14]=[N:13]1)([CH3:11])([CH3:9])[CH3:10]

Participants

5

Reactant 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 19081411HCID 19081411, compound

Product 1

HCID 23203297HCID 23203297, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Into 3 ml of a trifluoroacetic acid solution of 0.22 g of 2-tert-butyl-4-(4-methyl-1,3-dioxan-2-yl)-5-(4-pyridylmethylamino)pyridazin-3-(2H)-one obtained in Preparation Example 4 (2), 0.5 ml of deionized water was thoroughly dropwise added at room temperature. The mixture was stirred at room temperature for one hour. Then, 80 ml of ethyl acetate was added to the system, and the mixture was washed with a saturated sodium chloride aqueous solution. Then, the ethyl acetate layer was dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was subjected to column chromatography, and using an eluent (ethyl acetate:methanol=40:1), 0.15 g of the desired product (Compound No. 24) having a melting point of from 90° to 93° C. was obtained.

Workup

  1. additionwas thoroughly dropwise added at room temperature
  2. washthe mixture was washed with a saturated sodium chloride aqueous solution
  3. dry with materialThen, the ethyl acetate layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. customof from 90° to 93° C.
  6. customwas obtained

Sources & evidence

ORD record
ord-926f258efb054d2aa31180d973e030ae
Source dataset
uspto-grants-1998_06
Patent number
US05763439

Reaction notes

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