Water → HCID 54188526, compound

HRID 654703Notes

Reaction equation

HRID 654703 reaction equation
[CH2:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](O)=[C:8]([O:14][CH3:15])[CH:7]=[CH:6]2)[CH3:2].C[O:17][CH:18](Cl)Cl.[OH2:21]>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[CH2:1]([C:3]1[CH:4]=[C:5]2[C:10]([CH:9]=[C:8]([O:14][CH3:15])[C:7]([OH:21])=[C:6]2[CH:18]=[O:17])=[CH:11][CH:12]=1)[CH3:2]

Participants

6

Reactant 3

HCID 962WaterHCID 21004Methane, dichloromethoxy-HCID 14986469HCID 14986469, compound

Product 1

HCID 54188526HCID 54188526, compound

Reagents, catalysts & solvents 2

HCID 24193Titanium TetrachlorideCatalystHCID 6344DichloromethaneSolvent

Conditions

Temperature
0 °C

Procedure

3.3 g of 6-ethyl-2-methoxy-1-naphthol was dissolved in 25 ml of dichloromethane and cooled to 0° C. 3.65 ml of titanium tetrachloride and 2.4 ml of dichloromethyl methyl ether were added successively at that temperature and stirred for 10 min. After the reaction was over, water was added and the solution was extracted with ethyl acetate. After washing the extract with an aqueous saturated solution of sodium chloride, it was dried over anhydrous magnesium sulfate. When the solvent was distilled off and deposited crystals were washed with isopropyl ether, 2.5 g of the above-captioned compound was obtained as brown crystals.

Workup

  1. additionwas added
  2. extractionthe solution was extracted with ethyl acetate
  3. washAfter washing the
  4. extractionextract with an aqueous saturated solution of sodium chloride, it
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. distillationWhen the solvent was distilled off
  7. washwere washed with isopropyl ether

Sources & evidence

ORD record
ord-073df16e70aa487786804dbbea8be6a0
Source dataset
uspto-grants-1992_07
Patent number
US05134111

Reaction notes

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