Formic Acid → HCID 54105471, compound

HRID 1731490Notes

Reaction equation

HRID 1731490 reaction equation
[CH:1]1([CH:7]([OH:9])[CH3:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH:10](O)=[O:11]>>[CH:10]([O:9][CH:7]([CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH3:8])=[O:11]

Participants

3

Procedure

A mixture of 12.8 g. (0.1 moles) 1-cyclohexyl-1-ethanol and 13.8 g. (0.3 moles) formic acid was refluxed for two hours and then cooled to room temperature. It was poured in 200 ml. cold water, the organic material extracted in ether and the ether extract washed thoroughly with water, sodium bicarbonate, water and brine and dried over molecular sieves. 15.4 g. crude product of 97.9% purity was recovered--major impurity is residual solvent. The crude product was distilled through a short Vigreux-column. The product is a mobile, colorless liquid, b.p. 94° C./16 mm., nD25 =1.4437. Yield 13.6 g.=87.1%, purity 99.2% (by GLC) of 1-cyclohexyl-1-ethyl formate.

Workup

  1. additionA mixture of 12.8 g
  2. additionIt was poured in 200 ml
  3. extractioncold water, the organic material extracted in ether
  4. extractionthe ether extract
  5. washwashed thoroughly with water, sodium bicarbonate, water and brine
  6. customdried over molecular sieves
  7. customcrude product of 97.9% purity was recovered
  8. distillationThe crude product was distilled through a short Vigreux-column

Sources & evidence

ORD record
ord-ab2d400cc0124d3fb34868673b01b5ec
Source dataset
uspto-grants-1986_11
Patent number
US04622221

Reaction notes

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