英语翻译1,3-Diethynyl[1.1.1]bicyclopentane (9).37 Warning:Thisco

英语翻译
1,3-Diethynyl[1.1.1]bicyclopentane (9).37 Warning:This
compound has exploded upon heating.27 Anhydrous NH3
(40 mL) was condensed into a flask containing NaNH2 (3.8 g,
0.097 mol) under stirring at -78 °C,and 12 (3.22 g,0.017 mol)
was added dropwise from a syringe.The reaction mixture was
stirred for 30 min at -60 °C,slowly warmed to -30 °C over
the course of 2 h,and refluxed for 3 h.Then,dry diethyl ether
(20 mL) was added dropwise,and the NH3 was allowed to
evaporate slowly through a bubbler filled with mineral oil.
More diethyl ether (100 mL) was added,and the slurry was
stirred for 30 min at room temperature.From an addition
funnel,aqueous HCl (2 M) was added slowly under continued
stirring until the excess NaNH2 was consumed,and the
aqueous layer was acidified.The two layers were separated,
and the aqueous layer was extracted with diethyl ether (3 \2
15 mL).The organic layers were combined,washed with
saturated aqueous Na2CO3 (2 \2 15 mL),and dried over
Na2SO4.The solution was gently concentrated at atmospheric
pressure and 45 °C.With a minimum amount of diethyl ether
left,the flask was connected to a sublimation tube cooled with
dry ice,and the product was sublimed under vacuum (0.5 Torr)
after the remaining diethyl ether had evaporated into a liquid
nitrogen trap.The product 9 was weighed in the tube and
subsequently rinsed with dry diethyl ether into a round-bottom
flask for storage:1.64 g,(85%),mp 65 °C (lit.37 65-67 °C).1H
NMR (CDCl3,300 MHz) ä 2.05 (s,2 H),2.31 (s,6 H).37

1,3 - Diethynyl [ 1.1.1 ] bicyclopentane （ 9 ） 0.37警告：此
爆炸复合后heating.27无水氨
（ 40毫升）是浓缩成一个瓶含有NaNH2 （ 3.8克,
0.097摩尔）下搅拌在-78 ° C时,和第12条（三点二二克,0.017摩尔）
是滴加从一个注射器.是的反应混合物
搅拌30分钟在-60 ° ç ,缓慢升温至-30 ℃以上
的过程中2小时,并回流3小时接着,干乙醚
（ 20毫升）是滴加和氨被允许
蒸发缓慢通过喷水式饮水口充满了矿物油.
更多乙醚（ 100毫升）加入,和泥浆是
搅拌30分钟在室温下.从另外
漏斗,水盐酸（ 2男）是下继续增加缓慢
搅拌,直至超过NaNH2消耗,和
水层酸化.两层分离,
和水层提取乙醚（ 3
15毫升） .层的有机结合,洗
饱和水碳酸钠（ 2月15日毫升） ,和干燥的
硫酸钠.解决的办法是轻轻地集中在大气
压力和45 °角最低数额乙醚
左,瓶子是连接到一个升华管冷却
干冰,产品是真空状态下升华（ 0.5子）
之后,剩下的乙醚已变成液体蒸发
氮陷阱.该产品9体重在管
随后冲洗干乙醚成轮底
瓶贮存：一点六四克,（ 85 ％ ） ,熔点65 ℃ （ lit.37 65-67 ℃ ） .氢
核磁共振（ CDCl3 ,300兆赫）在2月5日（秒,2小时） ,2.31 （秒,6小时） 0.37