叔丁基氯的合成.docVIP

叔丁基氯的合成 一、实验原理(experimental principle ) (CH3)3OH + HCl------ (CH3)3CCl + H2O 二、仪器与药品(Instruments and drug) 分液漏斗，铁架台，烧杯，铁夹、冷凝管、温度计、温度计套管、橡胶管、量筒、 (Points, Taiwan, the metal liquid funnel beaker, iron clip, condensing tubes, thermometer, thermometer casing, rubber hose, LiangTong,) 三、装置图( Device figure ) 四、实验步骤( Operational steps) 在100mL分液漏斗中，放置4.8mL叔丁醇和12.5mL浓盐酸。先勿塞住漏斗，轻轻旋摇1min，然后将漏斗塞紧，翻转后摇振2—3min。注意及时打开活塞放气，以免漏斗内压力过大，使反应物喷出。静置分层后分出有机相，依次用等体积的水、5％碳酸氢钠溶液、水洗涤。用碳酸氢钠溶液洗涤时，要小心操作，注意及时放气。产物经无水氯化钙干燥后，滤入蒸馏瓶中，在水浴上蒸馏。接受瓶用冰水浴冷却，收集48—52℃馏分，产量约3.5g。 ( In 100mL canister portion of liquid funnel placed 4.8 mL uncle butanol and 12.5 mL strong hydrochloric acid. First dont plugged funnel, gently spinning 1min, then will funnel wave after wave, spins plugged 2-3min vibration. Note must open the pistons put gas, lest funnel, or excessive pressure in experiment. Quiet place stratification with organic phase, which in turn ceded such volume of water, 5% sodium bicarbonate solution, water washing. When catharsis with sodium bicarbonate solution, beware operation, note timely put gas. Product after by calcium chloride anhydrous dry distillation, strain into water bottle on distillation. Accept bottles of ice water bath cooling, collect 48-52 ℃ fractions, yield about 3.5 g. )