HRID1421314

反应详情

EQUATION

反应方程式

HRID 1421314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.5-dichlorophthalic anhydride (0.91, 4.19 mmol) ard 3-amino-3-(4-methoxyphenyl)propionic acid in 10 mL acetic acid was stirred under nitrogen for 6 hours. The reaction was cooled and removed some of the solvent. The slurry was filtered and the solid was dried to afford 1.20 g (61%) of 3-(4,5-dichlorophthalimido)-3-(4-methoxyphenyl)propionic acid as a white powder. mp 182-185° C.; 1H NMR (DMSO-d6, 250 MHz)δ 8.19(s, 2H), 7.34 (d, 2H, J=8.7), 6.90 (d, 2H, J=8.7), 5.61(t, 1H, J=7.8), 3.72 (s, 3H), 3.50-3.20 (m, 2H), 13C NMR (DMSO-d6) δ 171.6, 165 8, 158.8, 137.6, 131.0, 130.4, 128.4, 125.4, 113.9, 55.1, 50.0, 35.8. Anal. Calcd for C18H14N2O7. Theoretical: pending

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. customremoved some of the solvent
  3. filtrationThe slurry was filtered
  4. customthe solid was dried