반응 #91558

반응 방정식

Potassium tert-butoxide

1,1-dimethylethyl 7-(5-acetyl-2-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

Water

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title compound

1,1-dimethylethyl 7-[5-acetyl-2-({[4-(ethyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

용매

ethanol

반응 조건

후처리

1. 1
   온도this was heated in a microwave at 110 C
2. 2
   추출this was extracted with DCM (2×30 ml)
3. 3
   세척The combined organics were washed with brine
4. 4
   건조dried over sodium sulphate
5. 5
   농축concentrated in vacuo
6. 6
   기타The crude product was purified through silica eluting with 0-45% ethyl acetate in hexane

실험 절차

Potassium tert-butoxide (0.132 g) in ethanol (4 ml) was stirred for 15 min before adding 1,1-dimethylethyl 7-(5-acetyl-2-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (0.4 g) and this was heated in a microwave at 110 C. for 1.5 h. Water (20 ml) was added to the cooled mixture and this was extracted with DCM (2×30 ml). The combined organics were washed with brine, dried over sodium sulphate and concentrated in vacuo. The crude product was purified through silica eluting with 0-45% ethyl acetate in hexane to give the title compound, 0.16 g

출처