Hydrochloric Acid → HCID 22186476, compound

HRID 1795312Notes

Reaction equation

HRID 1795312 reaction equation
[CH:1]1([CH:7]2[CH2:12][CH2:11][CH2:10][CH2:9][CH:8]2O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:14]=[O:15].[ClH:16]>C(Cl)(Cl)Cl>[Cl:16][CH2:14][O:15][CH:12]1[CH2:11][CH2:10][CH2:9][CH2:8][CH:7]1[CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

5

Reactant 3

HCID 313Hydrochloric Acid2×HCID 712Formaldehyde2×HCID 943272-Cyclohexylcyclohexanol

Product 1

HCID 22186476HCID 22186476, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Conditions

Temperature
2.5 °C

Procedure

A 500 ml reactor made of glass was substituted by nitrogen, 46.6 g of 2-cyclohexylcyclohexanol and 200 ml of dehydrated chloroform were charged therein, and the resultant solution was stirred by a stirrer, and then 7.70 g of paraformaldehyde was added therein at the time of complete dissolution. Next, the reactor was cooled to 0 to 5° C. by ice bath, and hydrogen chloride was introduced into the solution by a bubbler. When a suspension of the solution caused by paraformaldehyde became clear and the solution became transparent, the introduction of hydrogen chloride was stopped. The lower phase was separately isolated, followed by drying by adding 28.3 g of anhydrous calcium chloride powder. Thereafter, 48.0 g of chloromethyl(2-cyclohexylcyclohexyl)ether was obtained (the purity according to 1H NMR was 87%) after distillation of the solvent.

Workup

  1. customA 500 ml reactor made of glass
  2. additionwere charged
  3. dissolutionat the time of complete dissolution
  4. additionWhen a suspension of the solution
  5. customThe lower phase was separately isolated
  6. customby drying
  7. additionby adding 28.3 g of anhydrous calcium chloride powder

Sources & evidence

ORD record
ord-2dbe459adddd4ce59e44f7eec81126a0
Source dataset
uspto-grants-2006_04
Patent number
US07026416B2

Reaction notes

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