Water → HCID 21504754, compound

HRID 1288331Notes

Reaction equation

HRID 1288331 reaction equation
C([O:5][C:6]([C:8]1[O:9][C:10]2[C:18]([Cl:19])=[CH:17][C:16]3[C:20]4[CH:29]=[CH:28][C:27]([S:30]([OH:33])(=[O:32])=[O:31])=[CH:26][C:21]=4[C:22]([CH3:25])([CH3:24])[O:23][C:15]=3[C:11]=2[C:12](=[O:14])[CH:13]=1)=[O:7])CCC.O>C(O)(=O)C.Cl>[C:6]([C:8]1[O:9][C:10]2[C:18]([Cl:19])=[CH:17][C:16]3[C:20]4[CH:29]=[CH:28][C:27]([S:30]([OH:33])(=[O:32])=[O:31])=[CH:26][C:21]=4[C:22]([CH3:25])([CH3:24])[O:23][C:15]=3[C:11]=2[C:12](=[O:14])[CH:13]=1)([OH:7])=[O:5]

Participants

5

Reactant 2

HCID 962WaterHCID 21504749HCID 21504749, compound

Product 1

HCID 21504754HCID 21504754, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 313Hydrochloric AcidSolvent

Procedure

1.0 gm (2 millimols) of 2-(n-butoxycarbonyl)-4-oxo-6,6-dimethyl-8-sulfo-12-chloro-4H,6H-[2]-benzopyrano-[3,4-f]-[1]-benzopyran (see Example 11) was heated for 1 hour in a mixture of 12 ml of acetic acid and 5 ml of concentrated hydrochloric acid. Then, the reaction mixture was evaporated to dryness, and the residue was recrystallized from methanol. 0.5 gm (53% of theory) of the compound named in the heading, m.p. 257°-259° C, was obtained (with 2 mols of water of crystallization).

Workup

  1. customThen, the reaction mixture was evaporated to dryness
  2. customthe residue was recrystallized from methanol
  3. customwas obtained

Sources & evidence

ORD record
ord-02dd3947f2c6472e9a457010bb3b7767
Source dataset
uspto-grants-1976_10
Patent number
US03987186

Reaction notes

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