Water → HCID 53968588, compound

HRID 2397280Notes

Reaction equation

HRID 2397280 reaction equation
[OH2:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][CH3:15])[C:10]([CH3:21])([CH2:16][CH2:17][C:18]([OH:20])=[O:19])[O:9][CH2:8][CH2:7]2>C(O)(=O)C.[O-2].[O-2].[O-2].[Cr+6]>[CH3:2][O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][CH3:15])[C:10]([CH3:21])([CH2:16][CH2:17][C:18]([OH:20])=[O:19])[O:9][CH2:8][C:7]2=[O:1]

Participants

5

Reactant 2

HCID 962Water2×HCID 12225887HCID 12225887, compound

Product 1

HCID 53968588HCID 53968588, compound

Reagents, catalysts & solvents 2

HCID 10219390chromium (VI) trioxideCatalystHCID 176Acetic AcidSolvent2×

Procedure

A solution of chromium trioxide (25.7 g) is a mixture of acetic acid (120 ml) and water (35 ml) is added dropwise to a solution of 6,7-dimethoxy-1-methylisochroman propionic acid (27.0 g), described in Example 16, in acetic acid (140 ml) keeping the temperature of the mixture below 20° C. The mixture is kept at room temperature for 1.5 hr. and then poured into water and extracted with chloroform. The extracts are thoroughly washed with water, dried and evaporated. The residue is crystallized from benzene to give the title compound, m.p. 172° - 173° C.

Workup

  1. customthe temperature of the mixture below 20° C
  2. extractionextracted with chloroform
  3. washThe extracts are thoroughly washed with water
  4. customdried
  5. customevaporated
  6. customThe residue is crystallized from benzene

Sources & evidence

ORD record
ord-a2f4bb207930451dad6946f1d1d5708a
Source dataset
uspto-grants-1977_05
Patent number
US04021451

Reaction notes

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