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HRID30969

反应详情

EQUATION

反应方程式

HRID 30969 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：CC(=O)OC(C)=O
HCID7918

Acetic anhydride

C4H6O3

结构：COC1(C)O[C@H](COCc2ccc(Cl)cc2Cl)[C@@H](OCc2ccc(Cl)cc2Cl)[C@H]1O
HCID69036486

未命名化合物

PRODUCTS

生成物

1
结构：COC1(C)O[C@H](COCc2ccc(Cl)cc2Cl)[C@@H](OCc2ccc(Cl)cc2Cl)[C@H]1OC(C)=O
HCID69037254

未命名化合物

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：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

To the solution of raw oil from Step 2 above (173.6 g, 0.3600 mol) in 1.379 L pyridine, were added Ac2O (33.970 mL, 0.3600 mol) and DMAP (1.3766 g, 0.01127 mol). After 21 hours of stirring at room temperature 1.4 L H2O were added. The solution was acidified with 1.45 L concentrated HCL. The acidified product was extracted with EtOAc, dried with MgSO4 and concentrated in vacuo. The residue was isolated as 85.75 g (0.1636 mol) of clear oil.

WORKUP

后处理

  1. additionwere added
  2. concentrationconcentrated HCL
  3. extractionThe acidified product was extracted with EtOAc
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated in vacuo