HRID904947

反应详情

EQUATION

反应方程式

HRID 904947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30 g of Z-Val-Val-OMe (prepared as in Chem. Ber. 103, 788-798 (1970)) are dissolved in 250 ml of methanol and subjected to catalytic hydrogenation at pH 4 after adding methanolic hydrochloric acid and Pd-on-BaSO4. When the reaction is complete, the catalyst is filtered off and the filtrate is concentrated. The resulting oil is triturated with ether. The substance crystallizes after a little time. It is filtered off and rinsed with ether. The substance is hygroscopic and is dried over P2O5 in vacuo. Yield 18.8 g, melting point 153°. [α]D23 =+2.5° (c=1, in methanol).

WORKUP

后处理

  1. filtrationthe catalyst is filtered off
  2. concentrationthe filtrate is concentrated
  3. customThe resulting oil is triturated with ether
  4. customThe substance crystallizes after a little time
  5. filtrationIt is filtered off
  6. washrinsed with ether
  7. dry with materialis dried over P2O5 in vacuo
  8. custom[α]D23 =+2.5° (c=1, in methanol)