1-(4-Chlorophenyl)-3,3-dimethylbutan-1-one → HCID 14365372, compound

HRID 1111526Notes

Reaction equation

HRID 1111526 reaction equation
[SH2:1].[Na].[CH2:3]([C:8]([C:10]1[CH:15]=[CH:14][C:13](Cl)=[CH:12][CH:11]=1)=[O:9])[C:4]([CH3:7])([CH3:6])[CH3:5]>CN1CCCC1=O>[CH2:3]([C:8]([C:10]1[CH:15]=[CH:14][C:13]([SH:1])=[CH:12][CH:11]=1)=[O:9])[C:4]([CH3:7])([CH3:6])[CH3:5]

Participants

4

Reactant 2

HCID 144983941-(4-Chlorophenyl)-3,3-dimethylbutan-1-oneHCID 86586439Sodium hydrogen sulphide

Product 1

HCID 14365372HCID 14365372, compound

Reagents, catalysts & solvents 1

HCID 13387N-methyl-2-pyrrolidoneSolvent

Conditions

Temperature
140 °C

Procedure

18.5 g (0.2 mol) of sodium hydrogen sulphide (NaSH·H2O) in 100 ml of N-methylpyrrolidone are introduced and the water is removed by partial distillation with xylene. The mixture is cooled to 140° C., 21.05 g (0.1 mol) of 4-(neopentylcarbonyl)-chlorobenzene are added, and the mixture is further reacted at 160° C. for 3 hours and worked up as described in Example I-1 to give 14 g (70% of theory) of the desired product of boiling point: 110°-115° C./0.1 mbar.

Workup

  1. customthe water is removed by partial distillation with xylene
  2. customthe mixture is further reacted at 160° C. for 3 hours

Sources & evidence

ORD record
ord-ae307e7fe2c840a4b2038112f7f99327
Source dataset
uspto-grants-1990_12
Patent number
US04980510

Reaction notes

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