Thionyl Chloride → HCID 12800625, compound

HRID 67097Notes

Reaction equation

HRID 67097 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 acid (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 relfuxed 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. stirringwith stirring
  2. concentrationThe reaction mixture was concentrated
  3. additionn-hexane was added to the
  4. concentrationconcentrate
  5. customto crystallize it
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed with n-hexane

Sources & evidence

ORD record
ord-a2d12b16c3cb489c8033c21ce5266a88
Source dataset
uspto-grants-1982_08
Patent number
US04344944

Reaction notes

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