Calcium hypochlorite → HCID 22708344, compound

HRID 353246

Reaction equation

HRID 353246 reaction equation
[Cl:1][O-].[Ca+2].Cl[O-].[F:6][C:7]([F:21])([F:20])[O:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[O:17][CH2:16][CH2:15][C:14]2=[O:19]>O.C(O)(=O)C.C(#N)C.O>[Cl:1][C:11]1[CH:12]=[C:13]2[C:18](=[C:9]([O:8][C:7]([F:6])([F:20])[F:21])[CH:10]=1)[O:17][CH2:16][CH2:15][C:14]2=[O:19]

Participants

6

Reactant 2

HCID 24504Calcium hypochloriteHCID 22708350HCID 22708350, compound

Product 1

HCID 22708344HCID 22708344, compoundYield 87%

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 6342AcetonitrileSolventHCID 21899381Acetic acid--water (1/1)Solvent

Procedure

To a solution of calcium hypochlorite (15.4 g, 72.4 mmol) in water:acetic acid (65:5) was added a solution of 8-trifluoromethoxychroman-4-one (4.2 g, 18.1 mmol; from step (iv) above) in acetonitrile (20 mL), whereafter the reaction mixture was stirred overnight. The mixture was diluted with water and extracted with ether (3 times) and EtOAc (once). The combined organic layer was washed with water, dried (Na2SO4) and evaporated, yielding 4.2 g (87%) of the sub-tide compound.

Workup

  1. extractionextracted with ether (3 times) and EtOAc (once)
  2. washThe combined organic layer was washed with water
  3. dry with materialdried (Na2SO4)
  4. customevaporated

Sources & evidence

ORD record
ord-043020b1396d4c3b960816fe83620a9d
Source dataset
uspto-grants-2004_06
Patent number
US06750243B1

Linked notes

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