Thionyl Chloride → HCID 12800625, compound

HRID 1649127Notes

Reaction equation

HRID 1649127 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

6,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic cid (1.1 g) was dissolved in benzene (20 ml) and thionyl chloride (2 ml) 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 and dired to afford the desired product (980 mg).

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

Sources & evidence

ORD record
ord-0cf56ebae7b148f48865e04a9f747e51
Source dataset
uspto-grants-1983_11
Patent number
US04415567

Reaction notes

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