支部特色之我们都是化学人实验篇 叔丁基氯的合成
2011-12-14 22:11阅读:
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 don't
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.
)