Thionyl Chloride → HCID 12800625, compound

HRID 1105531Notes

Reaction equation

HRID 1105531 reaction equation
[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([C:23](O)=[O:24])[C:10]2=[O:26])=[O:5])[CH3:2].S(Cl)([Cl:29])=O>C1C=CC=CC=1>[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([C:23]([Cl:29])=[O:24])[C:10]2=[O:26])=[O:5])[CH3:2]

Participants

4

Reactant 2

HCID 24386Thionyl ChlorideHCID 128006246,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

Product 1

HCID 12800625HCID 12800625, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

The compound (1.1 g) of Example 2 was dissolved in 20 ml of benzene, and 2 ml of thionyl chloride was added dropwise at room temperature with stirring. Then, the mixture was refluxed with stirring. The reaction mixture was concentrated, and n-hexane was added to the concentrate to crystallize it. The resulting crystals were collected by filtration, washed with n-hexane an dried to afford 980 mg of the desired product.

Workup

  1. temperatureThen, the mixture was refluxed
  2. stirringwith stirring
  3. concentrationThe reaction mixture was concentrated
  4. additionn-hexane was added to the
  5. concentrationconcentrate
  6. customto crystallize it
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with n-hexane
  9. customan dried

Sources & evidence

ORD record
ord-a3de4c92a7694a8184dd3b85395835ca
Source dataset
uspto-grants-1982_01
Patent number
US04309354

Reaction notes

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