反应详情

A solution of 5.0 g (50.0 mmol) 2-amino-thiazole, 10.7 g (50.0 mmol) 5-(pyridine-2-yl-ethynyl)-thiophene-2-carbaldehyde, 7.0 g (50.0 mmol) (2,4,4-trimethylpentane-2-yl)-isocyanide and 1.0 ml of a 70% aq. perchloric acid in chloroform (25 ml) was heated to 50° C. while being stirred for 5 d. Dilution with DCM was subsequently performed and a 1 molar aq. Na2CO3 sol. was added. After 10 min of stirring at RT, the phases were separated. The aqueous phase was extracted with DCM. The collected organic phases were dried over Na2SO4, filtered and concentrated in a vacuum. 11.86 g (27.3 mmol, 55%) 6-(5-pyridine-2-ylethynyl)thiophene-2-yl)-N-(2,4,4-trimethylpentane-2-yl)imidazo[2,1-b]thiazole-5-amine was obtained by multiple crystallisation of the residue from AE.

1. stirringAfter 10 min of stirring at RT
2. customthe phases were separated
3. extractionThe aqueous phase was extracted with DCM
4. dry with materialThe collected organic phases were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in a vacuum