3-Chloroanisole → HCID 178490749, compound

HRID 1459052Notes

Reaction equation

HRID 1459052 reaction equation
[Cl-:1].[Mg+2:2].[Cl-].[K].Cl[C:6]1[CH:7]=[C:8]([O:12][CH3:13])[CH:9]=[CH:10][CH:11]=1>O1CCCC1>[CH3:13][O:12][C:8]1[CH:7]=[C:6]([Mg:2][Cl:1])[CH:11]=[CH:10][CH:9]=1

Participants

5

Reactant 3

HCID 178333-ChloroanisoleHCID 5360315Magnesium ChlorideHCID 5462222Potassium

Product 1

HCID 178490749HCID 178490749, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

2.04 g (21.4 mmole) magnesium chloride were placed in a 100 ml three-necked flask fitted with a reflux condenser, thermometer and dropping funnel and were covered with 50 ml tetrahydrofuran (THF). 0.82 g (21.0 mmole) of freshly cut potassium was added in portions and the mixture was heated under reflux for 90 minutes, with stirring. Thereafter, 3.05 g (21.4 mmole) 3-chloroanisole, dissolved in 20 ml THF, was added drop-wise with stirring over 30 minutes. After the addition was complete, the mixture was stirred for 20 hours at room temperature and the Grignard compound obtained was used for further reaction.

Workup

  1. customfitted with a reflux condenser
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 90 minutes
  4. additionwas added drop-wise
  5. stirringwith stirring over 30 minutes
  6. additionAfter the addition
  7. stirringthe mixture was stirred for 20 hours at room temperature
  8. customthe Grignard compound obtained
  9. customwas used for further reaction

Sources & evidence

ORD record
ord-85ed786bebe34a329beaedb6e9dade36
Source dataset
uspto-grants-1998_12
Patent number
US05852216

Reaction notes

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