【在 a***n 的大作中提到】 : 狗屎gateway, 运来的机器CD drive hinge broken,这个就算了 : 结果onboard audio is not working, 并且, vista每次都在三分钟内freeze : 装上xp 之后还是不行, 找乐个旧声卡, 装上就成了 : 这个是不是基本没戏了?
d*6
7 楼
Sorry I cannot type chinese here. The solvents need to be exquisitely dry in order to get a good yield. You can buy those anhydrous solvents (pyridine, dioxane, tributylamine and DMF) and dry them over newly activated molecular sieves. An alternative way is to redistill the solvents freshly before reaction. The phosphorylation reagents should be made under argon protection and stored under 4 degree C (salicyl phosphorochlorodite), and -20 degree C ( tributylammonium pyrophosphate), respectively. Once made, these could be stable for ca. 6 months (i put the bottles in a bigger bottle containing drierite). DMF and tributylamine are not miscible to each other, so remember to shake the pyrophosphate/DMF/tributylamine mixture well before you add to the phosphorochlorodite intermediate. I am not sure whether your tributylammonium pyrophosphate will be fine. But I probably will buy a new one if I were you. It is pretty cheap. Good luck with your reaction.
【在 a***n 的大作中提到】 : 狗屎gateway, 运来的机器CD drive hinge broken,这个就算了 : 结果onboard audio is not working, 并且, vista每次都在三分钟内freeze : 装上xp 之后还是不行, 找乐个旧声卡, 装上就成了 : 这个是不是基本没戏了?
p*r
10 楼
太感谢了!包子奉上。
【在 d********6 的大作中提到】 : Sorry I cannot type chinese here. : The solvents need to be exquisitely dry in order to get a good yield. : You can buy those anhydrous solvents (pyridine, dioxane, tributylamine and : DMF) and dry them over newly activated molecular sieves. : An alternative way is to redistill the solvents freshly before reaction. : The phosphorylation reagents should be made under argon protection and : stored under 4 degree C (salicyl phosphorochlorodite), and -20 degree C ( : tributylammonium pyrophosphate), respectively. Once made, these could be : stable for ca. 6 months (i put the bottles in a bigger bottle containing : drierite).
m*y
11 楼
汗,研究下.
【在 p*********g 的大作中提到】 : 小学好可爱,奔一个
s*2
12 楼
use P NMR to check the purity.
m*y
13 楼
老了...
【在 s**********8 的大作中提到】 : bso年轻.
s*2
14 楼
use P NMR to check the purity.
h*g
15 楼
17年前小学毕业? 真年轻啊
【在 m**y 的大作中提到】 : 今天看了17年前小学毕业的集体照, : 感觉时光飞逝啊,哈哈
p*r
16 楼
We do not have P NMR in house. I will have to rely on HPLC for purity check.
【在 s****2 的大作中提到】 : use P NMR to check the purity.
m*y
17 楼
Sorry,算错了,16年前小学毕业....汗...
【在 h*********g 的大作中提到】 : 17年前小学毕业? : 真年轻啊
s*2
18 楼
tributylammonium pyrophosphate is not UV active!
check.
【在 p*****r 的大作中提到】 : We do not have P NMR in house. I will have to rely on HPLC for purity check.
p*g
19 楼
啥可研究的?
【在 m**y 的大作中提到】 : 汗,研究下.
p*r
20 楼
Sorry I thought you were talking about monitoring the reaction.
【在 s****2 的大作中提到】 : tributylammonium pyrophosphate is not UV active! : : check.