t***m
发帖数: 114 | 1 【 以下文字转载自 Chemistry 讨论区 】
【 原文由 TGDDM 所发表 】
各位帮忙想想反应，
我的一个样品，表面有很多羟基，部分和酰氯反应以改善溶解性
现在我想找一个反应
1.能够和羟基反应
2.产物比酯类稳定，这样，我在碱性条件下水解脱保护，可以破坏酯而不会
破坏这个键。
我想过用卤代烷烃或者异氰酸酯，不过对他们不熟悉，查Beilstein
也查了半天，还是不确定的说:-(
或者能否用其他方法保护，(不用酰氯，NND,味道太大，每次还要重蒸) |
y****u
发帖数: 50 | 2 Alkylsilyl group is the most popular.
the precursor could be alkylsilyl chloride.
it can be deprotected under more rigorous conditions if you want.
【在 t***m 的大作中提到】
: 【 以下文字转载自 Chemistry 讨论区 】
: 【 原文由 TGDDM 所发表 】
: 各位帮忙想想反应，
: 我的一个样品，表面有很多羟基，部分和酰氯反应以改善溶解性
: 现在我想找一个反应
: 1.能够和羟基反应
: 2.产物比酯类稳定，这样，我在碱性条件下水解脱保护，可以破坏酯而不会
: 破坏这个键。
: 我想过用卤代烷烃或者异氰酸酯，不过对他们不熟悉，查Beilstein
: 也查了半天，还是不确定的说:-(
|
t***m
发帖数: 114 | 3 ffdt
我的就是一个交连硅球
表明是氯甲基，我将他们变成了羟甲基而已
【在 y****u 的大作中提到】
: Alkylsilyl group is the most popular.
: the precursor could be alkylsilyl chloride.
: it can be deprotected under more rigorous conditions if you want.
|
a***n
发帖数: 578 | 4 CH3OH
-[ Si ]-
is it what you got? Does this materials have a lot of porous?
Did you use STM to look at it?
ester may not dissociate under base condition.
【在 t***m 的大作中提到】
: ffdt
: 我的就是一个交连硅球
: 表明是氯甲基，我将他们变成了羟甲基而已
|
t***m
发帖数: 114 | 5 heihei, yes
with CH2OH attached.
it is actually should be porous consider its
rough surface which made the functional groups
did not distribute evenly at the surface
I only have some AFM images so far
【在 a***n 的大作中提到】
: CH3OH
: -[ Si ]-
: is it what you got? Does this materials have a lot of porous?
: Did you use STM to look at it?
: ester may not dissociate under base condition.
|
a***n
发帖数: 578 | 6 what is your purpose to synthesis it?
can you measure the dissociation temperature of this materials?
By the way, can you send me some? hehe.
【在 t***m 的大作中提到】
: heihei, yes
: with CH2OH attached.
: it is actually should be porous consider its
: rough surface which made the functional groups
: did not distribute evenly at the surface
: I only have some AFM images so far
|
a***n
发帖数: 578 | 7 again, what is the melting and degeneration temperature?
Ester can be formed under acid condition and will not dissociate under base
condition. So maybe you use ester as protective group. |
t***m
发帖数: 114 | 8 sorry
昨天太匆忙了没回，sorry ah
I actually want to obtain some special tempelates
with surface slightly modified.
for example, we crosslink the sphere more tightly.
thus we stand great chance to obtain paritles with size
of only several nanometers
still not test this, expected 200 or higher
heihei, I am not in states,
what kind of particle you want
【在 a***n 的大作中提到】
: what is your purpose to synthesis it?
: can you measure the dissociation temperature of this materials?
: By the way, can you send me some? hehe.
|
t***m
发帖数: 114 | 9 成醚反应已经试过
没有成功:-(
melting/degeneration还没有测
我们这里没有TGA/DSC :-(
【在 a***n 的大作中提到】
: again, what is the melting and degeneration temperature?
: Ester can be formed under acid condition and will not dissociate under base
: condition. So maybe you use ester as protective group.
|
t******l
发帖数: 3060 | 10 how you try the reaction?
that reaction should be easy.
is ur polymer dissolve in solvent?
since ur -OH group is not that steric hindered. the general mathod can be.
dissolve in Solvent like Acetonnitrile, add K2CO3, add such as 1-bromoHexane.
refluxing for 24h. that's it.
for more rigorous condition. u can use stronger base, like KtBuO. refluxing in
higher temp.
【在 t***m 的大作中提到】
: 成醚反应已经试过
: 没有成功:-(
: melting/degeneration还没有测
: 我们这里没有TGA/DSC :-(
|
a***n
发帖数: 578 | 11 Thanks.
what is difference between the stuff you synthesis and silica. are they same
thing?
base
【在 t***m 的大作中提到】
: 成醚反应已经试过
: 没有成功:-(
: melting/degeneration还没有测
: 我们这里没有TGA/DSC :-(
|
t***m
发帖数: 114 | 12 我合成了一个聚甘油
所以有很多羟基
硅的那个你有兴趣可以看
Macromolecules 1997, 30, 7568-7573
1994，27，6102－6105
【在 a***n 的大作中提到】
: Thanks.
: what is difference between the stuff you synthesis and silica. are they same
: thing?
:
: base
|
t***m
发帖数: 114 | 13 yes, i know,
when I react it with 对氯甲基苯乙烯之类的反应时候，就不灵了
还有很多其他反应
thanks
【在 t******l 的大作中提到】
: how you try the reaction?
: that reaction should be easy.
: is ur polymer dissolve in solvent?
: since ur -OH group is not that steric hindered. the general mathod can be.
: dissolve in Solvent like Acetonnitrile, add K2CO3, add such as 1-bromoHexane.
: refluxing for 24h. that's it.
: for more rigorous condition. u can use stronger base, like KtBuO. refluxing in
: higher temp.
|
