huagongshe.com
HRID1040295

反应详情

EQUATION

反应方程式

HRID 1040295 的结构方程式

REACTANTS

反应物

4
结构：O
HCID962

Water

H2O

结构：CCN=C=NCCCN(C)C.Cl
HCID2723939

1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

C8H18ClN3

结构：CC(C)(C)OC(=O)C(O)CN
HCID22707757

Propanoic acid, 3-amino-2-hydroxy-, 1,1-dimethylethyl ester

C7H15NO3

结构：CC(C)(C)OC(=O)N(C(=O)OC(C)(C)C)[C@@H](CCCCN)C(=O)O
HCID22792075

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N(C(=O)OC(C)(C)C)[C@@](CCCCN)(C(=O)OCCN)C(=O)OC(C)(C)C
HCID131730895

未命名化合物

收率 68%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)c1ccncc1
催化剂HCID14284

N,N-Dimethylpyridin-4-amine

C7H10N2

结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

PROCEDURE

实验过程

Di-Boc lysine (770 grams, 2.2 mol) was dissolved in dichloromethane (4 liters). Bocethanolamine (340 grams, 2.1 mol) was added to the solution, along with 4-dimethylaminopyridine (50 grams.) EDC-HCl (450 grams, 2.35 mol) was added and the mixture was allowed to stir overnight at room temperature. Water (2 liters) was added and the mixture was stirred for 30 minutes. The layers were separated, and the aqueous layer was extracted with dichloromethane. The combined organics were washed with saturated sodium bicarbonate, 1N HCl solution, and brine. Solvent was removed under reduced pressure to give an oil. Mass recovery was 770 grams (68% yield).

WORKUP

后处理

  1. additionwas added
  2. stirringthe mixture was stirred for 30 minutes
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with dichloromethane
  5. washThe combined organics were washed with saturated sodium bicarbonate, 1N HCl solution, and brine
  6. customSolvent was removed under reduced pressure
  7. customto give an oil