HRID841143

反应详情

EQUATION

反应方程式

HRID 841143 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from Step 2 (1.8 g, 2.4 mmol) was dissolved in tetrahydrofuran (10 mL), methanol (10 mL) and water (2 mL). Sodium hydroxide (0.192 g, 4.8 mmol) was added and the mixture stirred overnight at room temperature. The solution was concentrated in vacuo and the residue taken up in 0.1 M NaPO4 buffer (100 mL). The pH was brought to 6 by the addition of 1N HCl. The product was extracted three times with ethyl acetate. The ethyl acetate was washed twice with brine, dried over MgSO4, filtered and concentrated in vacuo to give a white powder; 1.3 g (74% yield). MS-APCI: M+1=732.

WORKUP

后处理

  1. concentrationThe solution was concentrated in vacuo
  2. additionThe pH was brought to 6 by the addition of 1N HCl
  3. extractionThe product was extracted three times with ethyl acetate
  4. washThe ethyl acetate was washed twice with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customto give a white powder