Good quality 1-Iodoheptane CAS 4282-40-0

Good quality 1-Iodoheptane CAS 4282-40-0

production method
1. First, catechol is reacted with phosphorous trichloride to make phenyl chlorophosphinate, which is then reacted with heptanol to give a phosphite as a colorless oil. 50.9 g (0.20 mol) of phosphite and 50.8 g (0.20 mol) of iodine were added to 500 ml of methylene chloride and stirred at room temperature for 1 hour. Use 10% sodium thiosulfate solution to wash away any unreacted iodine that may be present, and wash sequentially with 5% NaOH solution, 5% NaHCO3 solution, and saturated NaCl solution. Separate the organic phase and evaporate the solvent. Distillation, collecting 96-104 ° C (5.33-6.4kPa) fractions, to obtain 39g of iodoheptane, the yield of 86%.
2. Preparation method: In a reaction flask equipped with a stirrer, reflux condenser and dropping funnel, add 110 g (1.0 mol) of catechol, cool in a water bath, and add phosphorus trichloride 206 g in 15 min under vigorous stirring. (1.5 mol), hydrogen chloride gas escaped continuously, and the reaction system gradually solidified. Stop stirring and let stand for 1 h at room temperature. The water bath was heated to melt and the reaction was stirred for 2 h. Vacuum distillation, accept the bottle with acetone – dry ice cooling, collecting 98 °C/3.33kPa or 91 °C/2.399kPa fractions, to obtain 165g of chlorophosphite catechol esters, yield of 95%. Place in the refrigerator and cure, mp 30°C. Add the above chlorophosphite phthalate ester to a 2L reaction flask
(2) 87 g (0.5 mol) of dried pyridine 39.5 g (0.5 mol) and 500 mL of anhydrous ether, cooled to 0°C, slowly add heptyl alcohol 58.1g (0.5 mol) and 400 mL of anhydrous ether solution, and leave at room temperature. overnight. It is suction filtered and the filter cake is washed with diethyl ether. The filtrate and washings were combined and the ether was evaporated to give 127 g of a colorless oil phosphite. In a reaction flask equipped with a stirrer, 50.9 g (0.2 mol) of the above phosphite, 500 mL of dried methylene chloride, and 50.8 g (0.2 mol) of iodine were added, and the reaction was stirred at room temperature for 1 hour. In a separatory funnel, it was washed with 10% sodium thiosulfate to iodine-free hydrochloric acid, followed by successive washing with 5% sodium hydroxide, 5% sodium carbonate, and saturated sodium chloride solution. Dry over anhydrous sodium sulfate. The water bath was distilled out of the solvent to give crude 1-iodoheptane…
use
For organic synthesis.

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