1-Butanol → HCID 13315698, compound

HRID 1768445Notes

Reaction equation

HRID 1768445 reaction equation
[C:1]1(C)[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[K+].[CH2:11](Cl)[CH2:12][CH2:13][CH3:14].S(=O)(=O)(O)O.[CH2:21](O)CCC>O>[CH3:11][CH:12]([CH2:13][CH3:14])[CH2:21][O:7][C:6]1[CH:1]=[CH:2][CH:3]=[CH:4][CH:5]=1

Participants

7

Procedure

540 g (5.0 mol) o-cresol, 500 g n-butanol and 560 g (5.0 mol) 50% (m/m) potassium hydroxide solution are initially introduced and heated under reflux, the water being removed azeotropically. 463 g (5.0 mol) n-butyl chloride are then metered in under reflux in the course of 2 h, further water being cycled out. After metering, the reaction mixture is stirred for a further 2 h, cooled to 80° C., hydrolysed with 800 g water and adjusted to pH 4 with 50% (m/m) sulphuric acid. The phases are separated at 70° C. After distillation, 794 g product with a purity of 94% is obtained.

Workup

  1. temperatureheated
  2. temperatureunder reflux
  3. customthe water being removed azeotropically
  4. customThe phases are separated at 70° C
  5. distillationAfter distillation, 794 g product with a purity of 94%
  6. customis obtained

Sources & evidence

ORD record
ord-688e4604d16a41c59edcd63c5515e828
Source dataset
uspto-grants-2007_06
Patent number
US07235699B2

Reaction notes

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