HRID879239

反应详情

EQUATION

反应方程式

HRID 879239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

500 mg (1.99 mmol) of N-Boc-L-phenylalaninol were dissolved in 5 ml DMF and cooled down to 0° C. under argon atmosphere. Then 159 mg (3.98 mmol) of a 60% suspension of sodium hydride was added in liquid paraffin. The reaction composition then was stirred until completion of gas formation and then mixed with 260 μl (2.19 mmol) of benzyl bromide. The cooling bath was removed and the reaction composition stirred for 2 hours at RT. Afterwards, the batch was evaporated, the residue absorbed in ice water and the composition extracted with dichlormethane. The organic phase was washed with saturated saline, dried over magnesium sulphate and evaporated. The residue was purified by means of a preparative HPLC. The yield was 226 mg (33% o. th.) of the title compound.

WORKUP

后处理

  1. customThe cooling bath was removed
  2. stirringthe reaction composition stirred for 2 hours at RT
  3. customAfterwards, the batch was evaporated
  4. customthe residue absorbed in ice water
  5. extractionthe composition extracted with dichlormethane
  6. washThe organic phase was washed with saturated saline
  7. dry with materialdried over magnesium sulphate
  8. customevaporated
  9. customThe residue was purified by means of a preparative HPLC