Benmoxine synthesis
- Product Name:Benmoxine
- CAS Number:7654-03-7
- Molecular formula:C15H16N2O
- Molecular Weight:240.3
Yield:7654-03-7 99%
Reaction Conditions:
with nickel(II) triflate;1,1,1,3',3',3'-hexafluoro-propanol;1,3-bis(dicyclohexylphosphine)propane in tert-Amyl alcohol at 120; for 24 h;Inert atmosphere;Schlenk technique;Molecular sieve;Sealed tube;
Steps:
5 Example 5: Preparation of N '- (1-phenylethyl) -benzohydrazide
To a 10 mL Schlenk reaction tube was added Ni (OTf) 2 (2.9 mg, 0.008 mmol), 1,3-bis (dicyclohexylphosphine) propane (4.4 mg, 0.010 mmol)And t-amyl alcoholMixed solvent with hexafluoroisopropanol (1.2 mL, volume 1: 1) was added and stirred for 10 minutes. Benzohydrazide (55 mg, 0.4 mmol), 1-phenylethanol (98 mg, 0.8 mmol) and molecular sieves (100 mg) were added successively. The reaction tube was sealed and heated in a 120 ° C oil bath for 24 hours. After the reaction is stopped, it is cooled and the reaction solution is added directly Into a silica gel column, eluting with petroleum ether and ethyl acetate (3: 1 by volume) to obtain pure N '- (1-phenylethyl) -benzoic hydrazide,Yield 99%.
References:
CN107400057,2017,A Location in patent:Paragraph 0066; 0067; 0068; 0069; 0070
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