N-Acetyl-L-methionine synthesis
- Product Name:N-Acetyl-L-methionine
- CAS Number:65-82-7
- Molecular formula:C7H13NO3S
- Molecular Weight:191.25
Yield:65-82-7 85.5%
Reaction Conditions:
with dicobalt octacarbonyl;carbon monoxide;hydrogen in 1,4-dioxane at 68 - 72; under 97509.8 Torr; for 5.5 h;Time;Concentration;
Steps:
1 Example 1
Example 1 [0030] To a stainless reactor equipped with a thermocouple, a stirrer, a gas supply line and a liquid supply line, 5.40 g (0.016 mol) of octacarbonyl dicobalt(0)[Co2(CO)8] and 39.86 g of 1,4-dioxane (38.7% by weight relative to a total amount of 1, 4-dioxane) were placed and stirred, and a mixed gas of carbon monoxide and hydrogen [carbon monoxide/hydrogen=2.3/1 (molar ratio)] was introduced to a gas phase portion in the reactor such that pressure in the reactor became 13 MPa (gauge pressure). Then, a temperature in the reactor was elevated to 68-72° C. while stirring was continued. At this time, pressure in the reactor was 13 MPa (gauge pressure). Then, to the reactor, a mixed solution of 31.57 g (0.30 mole) of 3-(methylthio)propionaldehyde [a compound represented by the formula (2) wherein R1 is a 2-thiomethoxyethyl group], 18.08 g (0.30 mole) of acetamide [a compound represented by the formula (3) wherein R2 is a methyl group and R3 is a hydrogen atom], 63.14 g of 1,4-dioxane (61.3% by weight relative to a total amount of 1,4-dioxane) and 5.40 g of water was added dropwise over 1.5 hour. After addition, the temperature in the reactor was held at 68-72° C. for 4 hours while stirring was continued, and then it was cooled to 5-35° C. to obtain 158.3 g of an acetyl methionine solution in 1,4-dioxane. A liquid chromatography analysis of the solution revealed that a yield of acetyl methionine relative to 3-(methylthio)propionaldehyde was 85.5%.
References:
US2013/116469,2013,A1 Location in patent:Paragraph 0030
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