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HRID246922

反应详情

EQUATION

反应方程式

HRID 246922 的结构方程式

REACTANTS

反应物

4
结构：O=N[O-]
HCID946

Nitrite ion

NO2-

结构：CCN(C(C)C)C(C)C
HCID81531

Diisopropylethylamine

C8H19N

结构：C1COCCO1.Cl
HCID20443148

1,4-Dioxane hydrochloride

C4H9ClO2

结构：CC[C@H](C)[C@H](NC(=O)OC(C)(C)C)C(=O)N[C@@H](Cc1ccccc1)C(=O)N[C@H](C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CO)C(=O)NN)[C@@H](C)O
HCID131714604

未命名化合物

PRODUCTS

生成物

1
结构：CC[C@H](C)[C@H](NC(=O)OC(C)(C)C)C(=O)N[C@@H](Cc1ccccc1)C(=O)N[C@H](C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CO)C(=O)N=[N+]=[N-])[C@@H](C)O
HCID131714607

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CS(C)=O
溶剂HCID679

Dimethyl sulfoxide

C2H6OS

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

3 次

CONDITIONS

反应条件

温度
-25 °C

PROCEDURE

实验过程

5.94 g (8.55 mM) of Boc-Ile-Phe-Thr-Asn-Ser-NH-NH2 are dissolved in 27 ml of DMSO plus 37 ml of DMF. After cooling to -25° C., 6.1 ml of a 5.6 N HCl/dioxane solution then 1.23 ml of tertiobutyl nitrite (1.2 equiv.) prediluted in 5 ml of DMF precooled to -20° C., are added. After 1 hr. 15 mins. of stirring between -20° and -25° C., 6.1 ml of diisopropylethylamine (DIPEA) are added to take the pH to around 6, then 3 ml of DMF are added to take the volume to 85 ml and this solution is conserved at -25° C.

WORKUP

后处理

  1. customprecooled to -20° C.
  2. additionare added
  3. custom15 mins
  4. customis conserved at -25° C.