Sulfuric Acid → HCID 21427683, compound

HRID 437996

Reaction equation

HRID 437996 reaction equation
S(=O)(=O)(O)O.[CH2:6]([C:8]1(O)[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH3:15])[CH3:7].[CH3:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][SH:23]>O>[CH2:6]([C:8]1([S:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH3:17])[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH3:15])[CH3:7]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 81061-HexanethiolHCID 2474821,2-Diethylcyclohexanol

Product 1

HCID 21427683HCID 21427683, compoundYield 76%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
0 °C

Procedure

To a cooled (0° C.) mixture of water (13 ml.) and 27 mg. concentrated sulphuric acid was added dropwise 1,2-diethylcyclohexanol (12 g., 77 mmole) and then n-hexylthiol (9.1 g., 77 mmole). The mixture was stirred at 0° C. for 6 hours and at room temperature for 1 hour. The mixture was then poured into 1 liter of cold water and extracted with ether. The ether extract was washed with 2N sodium hydroxide and water and dried (MgSO4). The solvent was removed by distillation and the residue was distilled under reduced pressure to give n-hexyl 1,2-diethylcyclohexyl sulphide (15 g.) as a colourless liquid, b.p. 110°-4°/0.03 mm.

Workup

  1. temperatureTo a cooled
  2. extractionextracted with ether
  3. extractionThe ether extract
  4. washwas washed with 2N sodium hydroxide and water
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed by distillation
  7. distillationthe residue was distilled under reduced pressure

Sources & evidence

ORD record
ord-67e7afc088a64bae962efaad97f1f6cf
Source dataset
uspto-grants-1977_06
Patent number
US04032661

Linked notes

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