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HRID1903342

反应详情

EQUATION

反应方程式

HRID 1903342 的结构方程式

REACTANTS

反应物

4
结构：C(=NC1CCCCC1)=NC1CCCCC1
HCID10868

Dicyclohexylcarbodiimide

C13H22N2

结构：On1nnc2ccccc21
HCID75771

1-Hydroxybenzotriazole

C6H5N3O

结构：CC(C)(C)OC(=O)N[C@@H](Cc1ccccc1)C(=O)N[C@H](Cc1c[nH]c2ccccc12)C(=O)N[C@@H](CCCCNC(=O)OCc1ccccc1)C(=O)O
HCID13391310

未命名化合物

结构：Cc1ccc(CSC[C@H](NC(=O)[C@@H](N)[C@@H](C)O)C(=O)N[C@H](CO)[C@@H](C)O)cc1.O=C(O)C(F)(F)F
HCID131713418

未命名化合物

PRODUCTS

生成物

1
结构：Cc1ccc(CSC[C@H](NC(=O)[C@@H](NC(=O)[C@H](CCCCNC(=O)OCc2ccccc2)NC(=O)[C@@H](Cc2c[nH]c3ccccc23)NC(=O)[C@H](Cc2ccccc2)NC(=O)OC(C)(C)C)[C@@H](C)O)C(=O)N[C@H](CO)[C@@H](C)O)cc1
HCID131713420

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

2 次

结构：CCN(CC)CC
溶剂HCID8471

Triethylamine

C6H15N

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2.5 ml NEt3, 11.2 g BOC-Phe-(D)Trp-Lys(Z)-OH and 4 g HOBT are added to 9 g H-Thr-Cys(MBzl)-Thr-ol trifluoroacetate in 100 ml DMF. 3.7 g DCCI in 10 ml DMF are added to the solution at -20° C. and the whole is stirred for ca. 18 hours at 0° C. and 2 hrs. at room temperature. Precipitated dicyclohexyl-urea is filtered off and the filtrate concentrated under vacuum and diluted with methanol. H2O is added until the product precipitates. The precipitate is filtered, washed with MeOH/H2O (4:1) and dried to yield the title compound:

WORKUP

后处理

  1. customat room temperature
  2. filtrationPrecipitated dicyclohexyl-urea is filtered off
  3. concentrationthe filtrate concentrated under vacuum
  4. additiondiluted with methanol
  5. additionH2O is added until the product
  6. customprecipitates
  7. filtrationThe precipitate is filtered
  8. washwashed with MeOH/H2O (4:1)
  9. customdried