ethyl 2.4-dioxo-4-p-tolylbutanoate synthesis
- Product Name:ethyl 2.4-dioxo-4-p-tolylbutanoate
- CAS Number:5814-37-9
- Molecular formula:C13H14O4
- Molecular Weight:234.25
Yield:5814-37-9 92%
Reaction Conditions:
with potassium etoxide in toluene at 50 - 60; for 4 h;
Steps:
11.1; 12.1; 13.1; 14.1 Example 11, Synthesis of 5-(4-methylbenzoyl)-2-hydroxypyrimidine
(1) In a 250 ml three-necked flask,Add 24 g (0.348 mol) of sodium ethoxide and 200 mL of dry toluene.Stir,Add dropwise (30 minutes dropwise) 45.6g (0.34mol)Uniform mixing of 4-methylacetophenone and 51.0 g (0.348 mol) of diethyl oxalateThe solution is heated to 50 to 60 ° C after the dropwise addition.The reaction was stirred for 4 h.Cool to room temperature,Wash with 5% dilute hydrochloric acid solution,And adjust the PH value to 5 to 6,Liquid separation,Collecting the toluene layer,Dry with anhydrous sodium sulfate for 30 minutes.filter,The filtrate pump is distilled under reduced pressure to recover toluene.The residue was recrystallized from 95% ethanol to give Intermediate 1 (purity: 99.1%) 73.3 g.The yield was 92%.
References:
CN108148003,2018,A Location in patent:Paragraph 0144; 0145; 0150; 0151; 0156; 0157; 0162; 0163
104-87-0
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