DI-TERT-BUTYL 1-(TERT-BUTYLTHIO)-1,2-HYDRAZINEDICARBOXYLATE synthesis

Yield:-

Reaction Conditions:

sodium ethanolate

Steps:

2 Preparation of 1tert.-butylthiohydrazine-1,2-dicarboxylic acid di-tert.-butyl ester

EXAMPLE 2 Preparation of 1tert.-butylthiohydrazine-1,2-dicarboxylic acid di-tert.-butyl ester A catalytic amount of sodium ethylate is added to a solution of 1.15 g. (0.005M) azodicarboxylic acid di-tert.-butyl ester and 0.57 ml. (0.005M) tert.-butylmercaptan in 20 ml. ether. The reaction proceeds exothermically. The solvent is removed in a vacuum and the oil residue is recrystallized from n-hexane. Yield 1.54 g. (96% of theoretical) Melting point 92°-96° C. C₁₄ H₂₈ N₂ O₄ S (320.45)--Theoretical: C 52.47, H 8.81, N 8.74, S 10.00. Actual: C 52.45, H 8.80, N 8.78, S 9.93.

References:

US4599407,1986,A