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HRID1154152

反应详情

EQUATION

反应方程式

HRID 1154152 的结构方程式

REACTANTS

反应物

5
结构：CCN1CCOCC1
HCID7525

N-Ethylmorpholine

C6H13NO

结构：C(=NC1CCCCC1)=NC1CCCCC1
HCID10868

Dicyclohexylcarbodiimide

C13H22N2

结构：On1nnc2ccccc21
HCID75771

1-Hydroxybenzotriazole

C6H5N3O

结构：CC(C)(C)Oc1ccc(C[C@H](NC(=O)OCc2ccccc2)C(=O)O)cc1
HCID978520

Z-TYR(TBU)-OH

C21H25NO5

结构：CCOC(=O)CNC(=O)[C@@H](N)Cc1ccc(OC(C)(C)C)cc1.Cl
HCID131714055

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=O)CNC(=O)[C@H](Cc1ccc(OC(C)(C)C)cc1)NC(=O)[C@H](Cc1ccc(OC(C)(C)C)cc1)NC(=O)OCc1ccccc1
HCID13178773

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

5.12 ml (40 mmoles) of N-ethylmorpholine and 8.65 g (42 mmoles) of DCC are added at 0° C. to a solution of 14.35 g (40 mmoles) of H-Tyr(But)-Gly-OEt.HCl, 14.84 g (40 mmoles) of Z-Tyr(But)-OH and 5.4 g (40 mmoles) of HOBt in 100 ml of dimethylformamide. The mixture is worked up as in Example 1 a. The residue is triturated with petroleum ether. Yield 26.3 g. The substance is purified by chromatographing a solution in 9:1 methylene chloride/acetone over 150 g of silica gel. The fractions were concentrated and the residue triturated with ether. Yield 19.74 g (73%), melting point 113°, [α]D22 =-28.7° (c=1, methanol).

WORKUP

后处理

  1. customThe residue is triturated with petroleum ether
  2. customThe substance is purified
  3. concentrationThe fractions were concentrated
  4. customthe residue triturated with ether
  5. customYield 19.74 g (73%), melting point 113°, [α]D22 =-28.7° (c=1, methanol)