HRID1656056

反应详情

EQUATION

反应方程式

HRID 1656056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 2-carboxy-2-[(acetylthio)methyl]-1,2,3,4-tetrahydronaphthalene (2.88 g, 10.0 mmol) in dry dimethylformamide (20 mL). To this solution add N-methyl morpholine (1.01 g, 10.0 mmol), isoserine benzyl ester tosylate salt (3.67 g, 10.0 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.92 g, 10.0 mmol). Stir the reaction mixture for 18 hours under an atmosphere of argon at ambient temperature then partition between ethyl acetate and dilute HCl. Wash the organic solution with water, saturated sodium hydrogen carbonate then brine. Dry the solution (MgSO4) and concentrate in vacuo. Purify the residue by column chromatography (ethyl acetate:hexane) to give the title compound.

WORKUP

后处理

  1. customthen partition between ethyl acetate and dilute HCl
  2. washWash the organic solution with water, saturated sodium hydrogen carbonate
  3. dry with materialDry the solution (MgSO4)
  4. concentrationconcentrate in vacuo
  5. customPurify the residue by column chromatography (ethyl acetate:hexane)