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HRID1838089

反应详情

EQUATION

反应方程式

HRID 1838089 的结构方程式

REACTANTS

反应物

4
结构：On1nnc2ccccc21
HCID75771

1-Hydroxybenzotriazole

C6H5N3O

结构：Cc1cccc(C)c1OCC(=O)O
HCID101369

Acetic acid, (2,6-dimethylphenoxy)- (9CI)

C10H12O3

结构：CCN=C=NCCCN(C)C.Cl
HCID2723939

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

C8H18ClN3

结构：COc1ccc(C[C@H](N)[C@H](O)C(=O)N2CSC(C)(C)[C@H]2C(=O)NC(C)(C)C)cc1
HCID69879176

未命名化合物

PRODUCTS

生成物

1
结构：COc1ccc(C[C@H](NC(=O)COc2c(C)cccc2C)[C@H](O)C(=O)N2CSC(C)(C)[C@H]2C(=O)NC(C)(C)C)cc1
HCID69878976

未命名化合物

收率 74.1%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

EDC-HCl (63 mg) was added to a solution of the compound obtained in Step 2 of Example 17 (127 mg), 2,6-dimethylphenoxyacetic acid (54 mg), and HOBt (41 mg) in DMF, and the mixture was stirred overnight. The reaction mixture was diluted with ethyl acetate, washed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl, dried over MgSO4, filtered and concentrated. The residue was purified by silica gel column chromatography and recrystallized from a mixture of EtOAc and n-hexane to obtain the title compound (130 mg).

WORKUP

后处理

  1. washwashed with 5% Na2CO3 (×2), 1N HCl, and 5% NaCl
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography
  6. customrecrystallized from a mixture of EtOAc and n-hexane