Chloral → HCID 13783049, compound

HRID 2210315Notes

Reaction equation

HRID 2210315 reaction equation
[CH2:1]([CH:3]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][OH:5])[CH3:2].[O:10]=[CH:11][C:12]([Cl:15])([Cl:14])[Cl:13]>C(CC(C)(C)C)(C)C.CC1C=C(OC)C=C(C)C=1.C(CC(C)(C)C)(C)C.Cl[Ti](Cl)(Cl)Cl>[CH2:1]([CH:3]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][O:5][CH:11]([OH:10])[C:12]([Cl:15])([Cl:14])[Cl:13])[CH3:2]

Participants

5

Reactant 2

HCID 6407ChloralHCID 77202-Ethylhexanol

Product 1

HCID 13783049HCID 13783049, compound

Reagents, catalysts & solvents 2

HCID 131719147HCID 131719147, compoundCatalystHCID 109072,2,4-TrimethylpentaneSolvent

Conditions

Temperature
-15 °C

Procedure

In a separate reaction vessel, the chloral 2-ethylhexyl hemiacetal was prepared from 1.05 g 2-ethyl-1-hexanol and 1.19 g (0.00807 mole) chloral substantially as described in Example 3. This material was dispersed in 1 ml of iso-octane and was added dropwise over twenty minutes to the 3,5-dimethylanisole/iso-octane/TiCl4 mixture. A sticky material precipitated, but the reaction solution was stirred at -15° C. for 4.5 hours before being with quenched with water, treated with NaOH, and worked-up substantially as described in Example 1.

Workup

  1. customIn a separate reaction vessel
  2. customA sticky material precipitated
  3. customwith quenched with water
  4. additiontreated with NaOH

Sources & evidence

ORD record
ord-3c0b3873e4a7432ca8e9373327eb4e0d
Source dataset
uspto-grants-1995_10
Patent number
US05457239

Reaction notes

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