ChemicalBook CAS DataBase List Methyl 4-Methoxy-5-(3-Morpholinopropoxy)-2-nitrobenzoate

Methyl 4-Methoxy-5-(3-Morpholinopropoxy)-2-nitrobenzoate synthesis

6synthesis methods

Product Name:Methyl 4-Methoxy-5-(3-Morpholinopropoxy)-2-nitrobenzoate
CAS Number:214472-37-4
Molecular formula:C16H22N2O7
Molecular Weight:354.36

214472-17-0
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Methyl 4-Methoxy-5-(3-Morpholinopropoxy)-2-nitrobenzoate

214472-37-4
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Yield:214472-37-4 92.3%

Reaction Conditions:

with sulfuric acid;nitric acid;sodium hydroxide in water;acetic acid at 5 - 20;

Steps:

II.1

(1) Preparation of methyl 2-nitro-4-methoxy-5-(3-morpholinopropoxy)benzoate 4 Methyl 4-methoxy-3-(3-morpholinopropoxy)benzoate 3 (43.5 g, 0.1408 mol) is dissolved in acetic acid (117 ml) at normal temperature, after moving to an environment with 5° C. for ten minutes, HNO₃ (21.75 ml, 45.5%) is added to react for 30 minutes, H₂SO₄ (44 ml, 70%) is added, and after cooled to room temperature, reaction is carried out for 2 hours. After reaction is completed, ice water (300 ml) is added at 5° C., water (170 ml) is used to wash a bottle with a rounded bottom, alkalinity is adjusted by adding NaOH (280 ml, 50%), stirring is carried out for 1 hours at a temperature less than 5° C., and extraction is performed by using ethyl acetate (770 ml) for twice. Extracts of ethyl acetate layer are combined, to be dried by MgSO₄, filtered, concentrated and dried for 16 hours to obtain daffadilly solid compound 4 (46 g, 92.3%).

References:

US2010/267949,2010,A1 Location in patent:Page/Page column 6