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CAS No. : | 1160250-95-2 | MDL No. : | MFCD12197963 |
Formula : | C14H9Cl3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 315.58 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With thionyl chloride; N,N-dimethyl-formamide In dichloromethane for 5h; Reflux; | 5.1.4.3. 4-(2,6-Dichlorobenzyloxy)benzoyl chloride (15) 14 (4.87 g, 0.016 mol) was dissolved in dry dichloromethane (60 mL). Then thionyl chloride (5.5 mL, 0.065 mol) and DMF (2 drops) were added to the mixture. The reaction mixture heated to reflux for 5 h and concentrated to give yellow solid 15 used for the next step without further purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
23.43% | In 1-methyl-pyrrolidin-2-one; at 20 - 25℃; | To a stirred solution of 18 (4 g, 0.016 mol) in 1-methyl-2-pyrrolidinone (60 mL) were added a solution of 15 in 1-methyl-2-pyrrolidinone (30 mL) at room temperature. The reaction mixture was stirred at 23-25 C overnight (12 h-18 h) and then diluted with ethyl acetate (100 mL). This solution was washed with water (2 × 100 mL) and then with 10% sodium hydrogen carbonate. The organic layer was dried, the solvent was evaporated in vacua. Purification of the crude products by column chromatography eluting with petroleum-ethyl acetate (2:1) gave 19 (1.5 g, 23.43%) as a white solid. Mp 198-200 C. 1H-NMR (300 MHz, CDCl3): 1.25-1.30 (t, J = 7.2 Hz, 3H, CH3), 4.17-4.25 (q, J = 7.2 Hz, 2H, CH2), 5.29 (s, 2H, CH2), 7.17-7.20 (d, J = 8.7 Hz, 2H), 7.37(s, 2H, NH2), 7.48-7.51 (t, J = 8.4 Hz, 1H, Ar), 7.57-7.60 (d, J = 7.2 Hz, 2H, Ar), 7.74-7.76 (d, J = 8.7 Hz, 2H); EI-MS (m/z): 406 (M)+. |