Application of 1280210-79-8, The chemical industry reduces the impact on the environment during synthesis 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, I believe this compound will play a more active role in future production and life.
INTERMEDIATE 6; 2-(2-Hydroxy-2-methylpropyl -2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-5-ium trifluoroacetate saltTo a stirred solution of tert-butyl 2,6-dihydropyrrolo[3 ,4-c]pyrazole-5(4H)-carboxyIate(35 g, 167 mmol) in DMF (500 mL) at 0 C under N2 was added sodium hexamethyldisilazide in THF (351 mL, 351 mmol) and the mixture was stirred at 0 C for 30 min. Isobutylene oxide (74.3 mL, 836 mmol) was then slowly added. The solution was stirred at 0C for 0.5 h and then stirred at room temperature for 1 h. The solution was heated to 80C for 100 min in a microwave oven, cooled to room temperature and evapoarted under vacuum. The residue was purified by column chromatography on silica gel, eluting with a gradient of 0% to 6% CH2Cl2 MeOH (containing 1 % NH4OH) to give a mixture of two regioisomers. The mixture of tworegioisomers A and B was resolved by chromatography on a ChiralPak AD-H column eluting with 4-40% MeOH/C02 to give isomer A as the faster eluting isomer and isomer B as the slower eluting isomer. NMR (500 MHz, CD3OD) for isomer B: 67.42 (d, 1 H); 4.42 (s, 2H); 4. 1 (s, 2H); 4.07 (s, 2H); 1.51 (d, 9H); 1.16 (s, 6H). LC-MS: 226.27 (M+l-56).The desired isomer B was treated with 1 :1 TFA/C?C12 for 1 h to give the title compound. NMR (500 MHz, CD3OD): 57.55 (s, 1H); 4.43 (s, 2H); 4.39 (s, 2H); 4.10 (s, 2H);1.17 (s, 6H). LC-MS: 182.31 (M+l).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, other downstream synthetic routes, hurry up and to see.