4-(DIMETHYL-13C 2-AMINO)ANTIPYRINE synthesis

Yield:60433-90-1 93%

Reaction Conditions:

Stage #1: 4-amino-2,3-dimethyl-1-phenylpyrazolin-5-onewith formic acid at 150; for 12 h;
Stage #2: [13C]-formaldehyde at 150; for 12 h;Temperature;Time;

Steps:

8 Example 8

The procedure is the same as Example 6,But the reaction time was changed to 12h and 12h, respectively.Yield 93%. Purity 99%Isotopic purity of 99%. The structural characterization results are the same as in Example 1.
To a 50 ml round bottom flask was added 1 g of 4-aminoantipyrine,1.33 g 85% formic acid,150 ° C for 4 h.Continue adding 0.48 g of 96% paraformaldehyde-13C,The reaction at 40 10h.After the end of the reaction, add sodium hydroxide and stir for 0.5h,Spin dry, extracted with n-hexane 3 times,Then recrystallized from ethanol,Activated charcoal in addition to color products.Yield 80%.Purity 99%.Isotopic purity of 99%.The structural characterization results are the same as in Example 1.

References:

CN106478509,2017,A Location in patent:Paragraph 0017; 0018; 0019; 0020; 0021; 0022; 0023-0041