p*****r
发帖数: 361 | 1 哪位大牛有经验？
以前没有做过这方面的反应。tributylammonium pyrophosphate有多稳定？标签上写的
是-20度保存。我拿到的时候已经在室温放了一两个月了。反应需要特别严格的无水条
件吗？ |
d********6
发帖数: 76 | 2 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 p*****r 的大作中提到】
: 哪位大牛有经验？
: 以前没有做过这方面的反应。tributylammonium pyrophosphate有多稳定？标签上写的
: 是-20度保存。我拿到的时候已经在室温放了一两个月了。反应需要特别严格的无水条
: 件吗？
|
p*****r
发帖数: 361 | 3 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).
|
s****2
发帖数: 4569 | 4 use P NMR to check the purity. |
s****2
发帖数: 4569 | 5 use P NMR to check the purity. |
p*****r
发帖数: 361 | 6 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.
|
s****2
发帖数: 4569 | 7 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*****r
发帖数: 361 | 8 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.
|
p****e
发帖数: 38 | 9 tributylammonium pyrophosphate是稳定的，只要干燥就行
【在 p*****r 的大作中提到】
: 哪位大牛有经验？
: 以前没有做过这方面的反应。tributylammonium pyrophosphate有多稳定？标签上写的
: 是-20度保存。我拿到的时候已经在室温放了一两个月了。反应需要特别严格的无水条
: 件吗？
|
p*****r
发帖数: 361 | 10 多谢！那为什么标签上要求-20度保存呢？
【在 p****e 的大作中提到】
: tributylammonium pyrophosphate是稳定的，只要干燥就行
|
p****e
发帖数: 38 | 11 标签上是要留margin保证可靠性的，有多科学就看生产者的良心了。但是低温保存肯定
不会错。不过我试过4度保存2个月，没有dessicate，没问题
我见过某公司的技术文档，基本上是拿别的公司的文档改了个公司图标...
【在 p*****r 的大作中提到】
: 多谢！那为什么标签上要求-20度保存呢？
|
