3,4-dihydro-2H-pyran → HCID 131734687, compound

HRID 1772848Notes

Reaction equation

HRID 1772848 reaction equation
[CH2:1]1[CH2:6][O:5][CH:4]=[CH:3][CH2:2]1.[Si:7]([Cl:11])([Cl:10])([Cl:9])[Cl:8]>C1(C)C=CC=CC=1>[Si:7]([Cl:11])([Cl:10])([Cl:9])[Cl:8].[CH2:1]1[CH2:6][O:5][CH:4]=[CH:3][CH2:2]1

Participants

4

Reactant 2

HCID 80803,4-dihydro-2H-pyran2×HCID 24816Silicon tetrachloride

Product 1

HCID 131734687HCID 131734687, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

DHP completely dissolved in 40 mL of toluene, yielding a yellow solution. SiCl4 was directly added to the DHP solution, immediately producing a very faint white cloudiness near the bottom of the flask. The mixture was stirred at ambient temperature for ˜72 hrs. A white precipitate was allowed to settle to the bottom of the flask. The solvent was removed under vacuum using a hot water bath. The yellow solution became increasingly dark as the solvent was removed; approximately 2-3 mL of liquid remained that would not evaporate. The remaining dark yellow slurry immediately turned brown upon air exposure. XRD analysis of the powder did not show any identifiable reflections.

Workup

  1. customyielding a yellow solution
  2. customimmediately producing a very faint white cloudiness near the bottom of the flask
  3. customThe solvent was removed under vacuum
  4. temperatureThe yellow solution became increasingly dark as the solvent
  5. customwas removed
  6. customevaporate

Sources & evidence

ORD record
ord-3cc1e7a03b1942ee8e9a395b02d0683f
Source dataset
uspto-grants-2016_02
Patent number
US09249505B2

Reaction notes

Loading…