4-Methylmorpholine synthesis
- Product Name:4-Methylmorpholine
- CAS Number:109-02-4
- Molecular formula:C5H11NO
- Molecular Weight:101.15
105-59-9
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$20.00/25g
109-02-4
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$10.00/5ml
Yield:109-02-4 98.4%
Reaction Conditions:
Stage #1: N-Methyldiethanolaminewith sulfuric acid at 60 - 170; for 7.5 h;
Stage #2: at 60 - 70; for 0.5 h;Temperature;Reagent/catalyst;Time;
Steps:
2 Example 2, a N-methyl morpholine cycle preparation method, N- methyl diethanolamine as raw material, concentrated sulfuric acid (concentration98%) as a catalyst, followed by the following steps:
1), synthesis:In a 500 ml four-necked flask, 120 g of concentrated sulfuric acid (1.2 mol, 98%) was slowly added dropwise (the temperature was controlled to not more than 60 ° C and the addition was completed in about 30 minutes) to 119.16 g of N-methyldiethanolamine The temperature was raised to 160 ~ 170 reflux reaction for 7 hours, during the reaction water was distilled off. After the reaction was completed, the mixture was cooled to room temperature to obtain a reaction solution.2), ammonium transfer:Under stirring at room temperature, 119.16 g of N-methyldiethanolamine (1 mol) was dropped into the reaction mixture (dropwise for about 30 minutes), and 2.38 g of T-5000 (about N-methylbis Ethanolamine 2% by mass), followed by raising the temperature to 60 to 70 ° C and stirring for 30 minutes.3) Distillation:The ammonium salt transfer reaction solution obtained in step 2) is subjected to vacuum distillation to collect 55-60 ° C. at a pressure of -0.95 MPaUnder a nitrogen atmosphere to obtain 99.63 g of N-methylmorpholine. Product purity of 99.9%; consumption of N-methyldiethanolamine as a benchmark,Yield 98.4%.
References:
CN106632143,2017,A Location in patent:Paragraph 0043; 0044; 0045; 0046; 0047; 0048; 0049-0092
7529-22-8
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109-02-4
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110-91-8
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124-38-9
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109-02-4
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109-02-4
466 suppliers
$10.00/5ml