반응 #481907
ord-865809982dde4a86acbf5c0e36b19187
반응 방정식
7-amino-4-(3-bromoanilino)-quinazoline
crotonic acid chloride
→
desired product
수율 31.2%
But-2-enoic acid [4-(3-bromo-phenylamino)-quinazolin-7-yl]-amide
수율 31.2%
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONWhen the addition
- 2기타the ice bath was removed
- 3여과The reaction was filtered
- 4기타to remove the yellow solid which
- 5세척was washed with tetrahydrofuran
- 6기타recrystallized from 20 mL of boiling methanol
실험 절차
To an ice cold solution of 0.158 g of 7-amino-4-(3-bromoanilino)-quinazoline (J Med Chem, 1985:3482) in 5 mL of tetrahydrofuran was added dropwise a solution of 0.105 g of crotonic acid chloride in 5 mL of tetrahydrofuran. When the addition was complete, the ice bath was removed and the reaction stirred at room temperature for 15 hours. The reaction was filtered to remove the yellow solid which was washed with tetrahydrofuran and recrystallized from 20 mL of boiling methanol to afford 0.060 g of the desired product, mp >250° C.