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HRID246915

反应详情

EQUATION

反应方程式

HRID 246915 的结构方程式

REACTANTS

反应物

2
结构：CC(C)(C)OC(=O)N[C@@H](CC(=O)OCc1ccccc1)C(=O)ON1C(=O)CCC1=O
HCID13517798

4-Benzyl 1-(2,5-dioxopyrrolidin-1-yl) N-(tert-butoxycarbonyl)-L-aspartate

C20H24N2O8

结构：CC[C@H](C)[C@H](NC(=O)OC(C)(C)C)C(=O)N[C@@H](CCSC)C(=O)NNC(=O)OCC(Cl)(Cl)Cl
HCID131714600

未命名化合物

PRODUCTS

生成物

1
结构：CC[C@H](C)[C@H](NC(=O)[C@H](CC(=O)OCc1ccccc1)NC(=O)OC(C)(C)C)C(=O)N[C@@H](CCSC)C(=O)NNC(=O)OCC(Cl)(Cl)Cl
HCID131714599

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

The preceding 30 g of oil in solution in 250 ml of THF are treated with 6.4 ml (50 mM) of NEM and 18.9 (45 mM) of Boc-Asp(OBzl)O Su. The apparent pH is adjusted between 6 and 7 by successive additions of NEM. After 4 hours, the product is isolated by evaporation of the THF, take-up in 400 ml of ethyl acetate followed by the same washings as the preceding homologue (3). The residue after drying and evaporation (36.5 g) is purified by chromatography over a column of silica with dichloromethane as solvent containing from 0 to 1.5% of methanol. 25 g (66%) of product presenting an NMR spectrum in accordance with the expected structure are thus obtained.

WORKUP

后处理

  1. customThe residue after drying
  2. customevaporation (36.5 g)
  3. customis purified by chromatography over a column of silica with dichloromethane as solvent
  4. additioncontaining from 0 to 1.5% of methanol
  5. customare thus obtained