반응 #43998

반응 방정식

2,3-bis(bromomethyl)-1,4-diethoxy-naphthalene

4-aminophenylacetic acid ethyl ester

→

product

수율 36.0%

Ethyl[4-(4,9-diethoxy-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate

수율 36.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The solvent was removed in vacuo
2. 2
   세척washed with 8% aqueous sodium bicarbonate solution (5 ml)
3. 3
   건조The organic layer was dried over magnesium sulphate
4. 4
   기타the solvent removed in vacuo
5. 5
   기타Purification by flash column chromatography on silica gel eluting with 90% cyclohexane/ethyl acetate

실험 절차

A solution of 2,3-bis(bromomethyl)-1,4-diethoxy-naphthalene (41 mg, 0.1 mmol) and 4-aminophenylacetic acid ethyl ester (20 mg, 0.11 mmol) in N,N-dimethylformamide (1 ml) was heated at 60° C. under nitrogen for 14 h. The solvent was removed in vacuo and the residue taken up in ethyl acetate (10 ml) and washed with 8% aqueous sodium bicarbonate solution (5 ml). The organic layer was dried over magnesium sulphate and the solvent removed in vacuo. Purification by flash column chromatography on silica gel eluting with 90% cyclohexane/ethyl acetate gave the product as a white solid (15 mg, 36%).

출처