4-Methyldiphenylamine synthesis
- Product Name:4-Methyldiphenylamine
- CAS Number:620-84-8
- Molecular formula:C13H13N
- Molecular Weight:183.25
Yield:620-84-8 92%
Reaction Conditions:
with nickel(II) chloride hexahydrate;triethylamine at 125; for 0.333333 h;Microwave irradiation;Neat (no solvent);
Steps:
General procedure for preparation of N-arylated amines 3: Aryl halide (1 mmol), amine (1.5 mmol), NiCl2·6H2O (10 mol % relative to aryl halide) and triethylamine (1.4 equiv) were taken in a 10 mL pressurized microwave vial with snap on cap. The reaction mixture was subjected to microwave exposure for 20 min at 300 W at appropriate temperature as indicated above. The progress of the reaction was monitored by TLC (Thin Layer Chromatography). After the reaction was completed, the reaction mixture was diluted with DCM and the insoluble catalyst was recovered and recycled without loss of activity. The filtrate was concentrated and subjected to column chromatography with n-hexane and ethyl acetate (2-10% depending upon the product) as eluent to afford the pure product.
References:
Gupta, Amit Kumar;Tirumaleswara Rao;Singh, Krishna Nand [Tetrahedron Letters,2012,vol. 53,# 17,p. 2218 - 2221] Location in patent:experimental part
