Sulfuric Acid → HCID 20334254, compound

HRID 1706713Notes

Reaction equation

HRID 1706713 reaction equation
[CH3:1][C:2](O)([CH2:4][CH:5](O)[CH3:6])[CH3:3].[CH2:9]([C:12]1[C:18]([OH:19])=[CH:17][C:16]([CH3:20])=[CH:15][C:13]=1[OH:14])[CH2:10][CH3:11].C(OC(C)C)(C)C.S(=O)(=O)(O)O>>[OH:19][C:18]1[C:12]([CH2:9][CH2:10][CH3:11])=[C:13]2[C:15]([CH:5]([CH3:6])[CH2:4][C:2]([CH3:3])([CH3:1])[O:14]2)=[C:16]([CH3:20])[CH:17]=1

Participants

5

Reactant 4

HCID 1118Sulfuric AcidHCID 7870Hexylene GlycolHCID 7914Diisopropyl EtherHCID 12529753HCID 12529753, compound

Product 1

HCID 20334254HCID 20334254, compoundYield 72.6%

Procedure

An amount of 1.77 g. of 2-methylpentane-2,4-diol were added dropwise at the temperature of approximately 60° C. to a mixed solution prepared from 2.49 g. of 2-propyl-5-methyl resorcinol, 15 ml of isopropyl ether and 1 ml of concentrated sulfuric acid. The solution was cooled, and successively washed with water, aqueous 1 N sodium hydroxide solution, and again with water, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by subjecting to column chromatography filled with silica gel. There were thus obtained 2.7 g. (yield: 72.6%) of the subject compound in oily form.

Workup

  1. customprepared from 2.49 g
  2. temperatureThe solution was cooled
  3. washsuccessively washed with water, aqueous 1 N sodium hydroxide solution
  4. dry with materialagain with water, and then dried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customThe residue was purified
  7. additionfilled with silica gel

Sources & evidence

ORD record
ord-0c8619963e9a4ec7b38edea450733b6c
Source dataset
uspto-grants-1980_06
Patent number
US04208426

Reaction notes

Loading…