Sodium Hydroxide → 105607-67-8

HRID 2308897Notes

Reaction equation

HRID 2308897 reaction equation
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][CH:5]=[C:6]([OH:10])[CH:7]=2)[O:2]1.[OH-].[Na+].S(Cl)([Cl:16])(=O)=O>C(OCC)C>[Cl:16][C:5]1[CH:4]=[C:3]2[O:2][CH2:1][O:9][C:8]2=[CH:7][C:6]=1[OH:10]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 24648Sulfuryl chlorideHCID 68289Sesamol

Product 1

HCID 19431144105607-67-8

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

To a solution of 0.18 mol (25 g) of 4,5-methylenedioxyphenol in 125 ml of ethyl ether, 17 ml of sulphuryl chloride are added at a temperature below 35° C. As soon as the addition is complete, the ethyl ether is evaporated off at room temperature. The dry residue thereby obtained is taken up with 2N sodium hydroxide. The mixture is filtered to remove a resin. The filtrate is acidified with 2N hydrochloric acid; the expected product precipitates. After being washed with water and dried under vacuum in the presence of phosphorus pentoxide, it is recrystallized from a cyclohexane/benzene mixture. It melts at 95° C.

Workup

  1. additionAs soon as the addition
  2. customthe ethyl ether is evaporated off at room temperature
  3. customThe dry residue thereby obtained
  4. filtrationThe mixture is filtered
  5. customto remove a resin
  6. customthe expected product precipitates
  7. washAfter being washed with water
  8. dry with materialdried under vacuum in the presence of phosphorus pentoxide, it
  9. customis recrystallized from a cyclohexane/benzene mixture

Sources & evidence

ORD record
ord-24fabe2e562546a1b3552136f49d05d4
Source dataset
uspto-grants-1987_09
Patent number
US04692166

Reaction notes

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