Sodium Sulfate → HCID 18990363, compound

HRID 1195958Notes

Reaction equation

HRID 1195958 reaction equation
C[O:2][C:3]1[CH:4]=[C:5]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])[C:6]([N+:11]([O-:13])=[O:12])=[CH:7][C:8]=1[O:9]C.[O-]S([O-])(=O)=O.[Na+].[Na+]>C(O)(=O)C.Br>[OH:2][C:3]1[CH:4]=[C:5]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])[C:6]([N+:11]([O-:13])=[O:12])=[CH:7][C:8]=1[OH:9]

Participants

5

Reactant 2

HCID 24436Sodium SulfateHCID 19389219HCID 19389219, compound

Product 1

HCID 18990363HCID 18990363, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 260Hydrogen BromideSolvent

Procedure

A solution containing 42.0 g of the product obtained in Example 40 in 100 ml of acetic acid and 150 ml of 48% hydrobromic acid was refluxed for 10 h. 1 l of saturated Na2SO4 -solution was added to the reaction mixture and extracted with ether. The solvent was evaporated in vacuo and the residue crystallized from ethyl acetate-petroleum ether. Yield 7.9 g (19%), m.p. 111°-114° C.

Workup

  1. temperaturewas refluxed for 10 h
  2. extractionextracted with ether
  3. customThe solvent was evaporated in vacuo
  4. customthe residue crystallized from ethyl acetate-petroleum ether

Sources & evidence

ORD record
ord-2d98bb707f4e44f3879b16b7c2085765
Source dataset
uspto-grants-1992_05
Patent number
US05112861

Reaction notes

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