반응 #76456

반응 방정식

dihydrophthalazine

4-(4-Acetylaminophenyl)-1,2-dihydro-1-methyl-6-methylthiophthalazine

ethyl isocyanate

→

desired products 9

수율 50.0%

4-(4-Acetylaminophenyl)-1,2-dihydro-1-methyl-2-ethylcarbamoyl-6-methylthiophthalazine

수율 50.0%

용매

chloroform

반응 조건

후처리

1. 1
   workup.WAITleft from TLC
2. 2
   기타The solvent was removed under reduced pressure
3. 3
   기타Purification of the crude product

실험 절차

To a solution of dihydrophthalazine 8 in chloroform was added ethyl isocyanate (3 eq) at room temperature. The resulting solution was stirred at such temperature for a few days until there is no starting material left from TLC. The solvent was removed under reduced pressure. Purification of the crude product by using a silica gel gave the desired products 9 (Yield: 50%). 1HNMR (CDCl3): 7.70-7.55 (m, 5H), 7.35 (dd, J=4.3 Hz, 1H), 7.19 (m, 2H), 6.53 (br, 1H), 5.73 (q, J=13.2 Hz, 1H), 3.42 (m, 2H), 2.40 (s, 3H), 2.25 (s, 3H), 1.22 (m, 6H).

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