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HRID1267569

反应详情

EQUATION

反应方程式

HRID 1267569 的结构方程式

REACTANTS

反应物

4
结构：CCN1CCOCC1
HCID7525

N-Ethylmorpholine

C6H13NO

结构：CCN=C=NCCCN(C)C.Cl
HCID2723939

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

C8H18ClN3

结构：O.On1nnc2ccccc21
HCID2796029

1H-Benzotriazol-1-ol--water (1/1)

C6H7N3O2

结构：CC(C)C[C@H](NC(=O)[C@H](CO)NC(=O)[C@@H](N)CCC(N)=O)C(=O)OCc1ccccc1.Cl
HCID69996228

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)C[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](CCC(N)=O)NC(=O)CNC1CCCCC1)C(=O)OCc1ccccc1.Cl
HCID69994356

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

3
结构：O
溶剂HCID962

Water

H2O

结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

N-(glutaminyl-serinyl)leucine benzyl ester hydrochloride (2.6 kg) (prepared as described in Step 3), N-Boc-L-cyclohexylglycine (1.414 kg) and HOBt hydrate (168 g) were dissolved in DMF (13.0 L). N-ethylmorpholine (1.266 kg, 11.0 M) and EDC hydrochloride (1.265 kg) were added and the mixture stirred at 20° C. for 3 hours. The solution was diluted with ethyl acetate (13.0 L) and water (26.0 L) added. The product precipitated and the slurry was stirred at room temperature for 1 hour. The solid was collected by filtration, washed with 1:1 ethyl acetate/water (60 L) dried on the filter under nitrogen for 24 hours and dried in vacuo at 45°. The title compound was obtained as a white solid.

WORKUP

后处理

  1. additionadded
  2. customThe product precipitated
  3. stirringthe slurry was stirred at room temperature for 1 hour
  4. filtrationThe solid was collected by filtration
  5. washwashed with 1:1 ethyl acetate/water (60 L)
  6. customdried on the
  7. filtrationfilter under nitrogen for 24 hours
  8. customdried in vacuo at 45°