ChemicalBook CAS DataBase List IODOMETHANE-D3

IODOMETHANE-D3 synthesis

5synthesis methods

Product Name:IODOMETHANE-D3
CAS Number:865-50-9
Molecular formula:CD3I
Molecular Weight:144.96

In an anhydrous and oxygen-free glove box under an argon atmosphere, add [Ir (COD) Cl]2 (0.001 mmol), PPh3 (0.002 mmol) and deuterated methanol (0.2 mmol) to the 10 mL pressure reaction. Into the tube, then add 1 mL of THF (tetrahydrofuran),Then add I2 (0.2 mmol) and send it out of the glove box, put it in the autoclave and fill it with 20 bar H2. The reaction was carried out in an oil bath at 20°C, and the reaction was detected in the gas phase. After the reaction was completed, the reaction was concentrated, and a colorless liquid deuterated methyl iodide was obtained through the column with silica gel. The yield was 88%.Then, NaH, D3I and (tert-butoxycarbonyl)-L-homocysteine methyl ester were dissolved in THF at a ratio of 2.2: 2:1 and stirred at room temperature for 3 hours to obtain product with a yield of 80%.

811-98-3
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865-50-9
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$25.00/1g

Yield:865-50-9 83.8%

Reaction Conditions:

with hydrogen iodide in water at 40 - 50; for 4 h;

Steps:

3 Example 3: CD3- iodomethane (Compound 5A) Synthesis
To the reaction flask was added 5mL deuterated methanol, water and 50mL 5mL percentage of hydriodic acid (mass55.0% -58.0%, by mass percentage, means the mass of hydrogen iodide accounts for the total mass percentage hydroiodicStabilizer mass% hypophosphorous acid containing 1.5%, by mass percentage, means hypophosphorous acid; division ratioStabilizer mass percentage of the total mass of hydroiodic acid reagent), followed by stirring, the reaction was heated to 40 2h,The reaction was heated to 50 deg.] C 2h, cooled to room temperature (about 20 deg.] C), into a distillation apparatus, atmospheric pressure (1 atm for),40 ~ 45 collected fractions, the distillation rate of 0.1mL / second to give 13.25 g of a colorless liquid, yield 83.8%.

References:

Shanghai Institute of Organic Chemistry;Ding, Wenhui;Long, Qin;Li, Xiaoqiang;Fang, Tong;Yang, Jun CN104557815, 2016, B Location in patent:Paragraph 0105; 0106; 0107

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