| production method | 1.?? Note that j is carried out in a fume hood. strong heat and rubber products are strictly prohibited. Place 80 grams (2 moles) of sodium hydroxide and 500ml of water in a 2-liter three-neck flask equipped with a stirrer, gas introduction tube and outlet tube. After the solid is dissolved, 74g (94 ml, 1 mol) of tert-butanol and about 500ml of water are added under 15-20 ℃ and uniform stirring. First, the chlorine gas is passed at a speed of 1 liter/minute for 30 minutes, and then the chlorine gas is passed at a speed of 0.5-0.6 liters/minute for 30 minutes (to). Separate the upper organic layer and wash it several times with 50ml of 10% sodium carbonate solution until the Congo red test paper no longer shows acidity. Wash with equal accumulation of water for 4 times, add anhydrous calcium chloride and dry to separate 78-107g (72-99%) of liquid product. Store in the refrigerator in the presence of inert gas away from light. 2. Attention! Operating in a dimly lit fume hood, it is strictly forbidden to contact the product with the rubber and the heating temperature exceeds its boiling point. In a 1-liter flask or round bottom flask equipped with a stirrer, add 500ml of sodium hypooxy solution containing 0.375-0.400 moles, then cool in an ice bath and stir quickly to reduce the temperature to below 10 ℃. Under dark and fast stirring, add 37ml of 0.39 mol) tert-butanol and 24.5ml (0.43 mol) glacial acetic acid in turn. After stirring for 3 minutes, transfer the reaction mixture to a 1 liter separatory funnel. Separate the underlying water layer. The oily yellow organic layer is first washed with 50ml of 10% sodium carbonate solution and then washed with 50ml of water. Add 1g of anhydrous calcium chloride, dry and filter to obtain a liquid product with a purity of 99-100%, weighing 29.6-34 (70-80%). Put it in a dark glass bottle with calcium chloride and store it in the refrigerator. 3. Preparation method: Heat 500mL(5% ~ 6%) of sodium hypochlorite solution in a reaction bottle equipped with a stirrer and a thermometer, cool it to below 10 ℃ in an ice bath, and cover the reaction bottle with black cloth to avoid strong light. Vigorously stir the solution prepared by adding 37mL(0.39mol) of tert-butanol (2) and 24.5mL(0.43mol) of glacial acetic acid, and continue stirring for 3min. The reaction solution is poured into a separatory funnel, and the water layer is separated. The yellow oily organic layer is washed with 50mL of 10% sodium carbonate solution and 50mL of water in turn. Anhydrous calcium chloride is dried and filtered to obtain 30-34g of tert-butyl hypochlorite (1) with a yield of 70%-80% and a purity of 99%-100%. Store in a brown bottle with calcium chloride desiccant in a refrigerator. [3] 4. Add 50mL of water and 80g(2.0mol) of sodium hydroxide to a reaction bottle equipped with a stirrer and a ventilation tube, stir and dissolve, cool until chlorine gas is introduced for 30min, and then chlorine gas is introduced at a speed of 0.5 ~ 0.6L per minute for 30min. Pour the reaction solution into a separatory funnel to separate the water layer. The yellow oily organic layer is washed with 50mL of 10% sodium carbonate solution at a time until it is no longer acidic to Congo red. Wash it with water for four times. Anhydrous calcium chloride is dried and filtered to obtain 78-107g of tert-butyl hypochlorite ① (1) with a yield of 72%-99%. Store in a brown bottle with calcium chloride desiccant and inert gas protection in a refrigerator. Note: ① The product contains about 2% free chlorine, which is sufficient for most purposes. It can be purified by distillation, bp77 ~ 78 ℃. Through the determination of active chlorine, the purity is 97% ~ 98% when it is not purified, and the purity after purification is 98% ~ 100%. [4] |
