R****n
发帖数: 708 | 1 我想用这个反应做个化合物物。这个反应会产生氮气，需要一个高效的反应条件。不是做有机的，可能问的比较白痴。谢谢！请看二楼附件 | R****n
发帖数: 708 | | h****z
发帖数: 1996 | 3 有相关paper吗
【在 R****n 的大作中提到】
: 反应在这里
| R****n
发帖数: 708 | 4 http://www.pnas.org/content/108/8/3270.figures-only
This is a biochem paper. The supplementary material mentioned how to convert
a Glutamate Acid to 2-Hydroxygluataric acid. But no detailed infor
Quote from the paper
(R)-2-hydroxyglutarate Synthesis. (R)-2-hydroxyglutarate (2HG) was
synthesized by treatment of D-glutamate (Sigma-Aldrich) with nitrous
acid to forma lactone, which was then hydrolyzed with NaOH
solution to form 2-D-hydroxylglutarate. Purity was 93%. Powder
was resuspended in PBS and filtered through a 0.22-μm filter using
sterile technique for treatment of cells.
【在 h****z 的大作中提到】
: 有相关paper吗
| s*******h
发帖数: 3731 | 5 ask the author ya...
convert
【在 R****n 的大作中提到】
: http://www.pnas.org/content/108/8/3270.figures-only
: This is a biochem paper. The supplementary material mentioned how to convert
: a Glutamate Acid to 2-Hydroxygluataric acid. But no detailed infor
: Quote from the paper
: (R)-2-hydroxyglutarate Synthesis. (R)-2-hydroxyglutarate (2HG) was
: synthesized by treatment of D-glutamate (Sigma-Aldrich) with nitrous
: acid to forma lactone, which was then hydrolyzed with NaOH
: solution to form 2-D-hydroxylglutarate. Purity was 93%. Powder
: was resuspended in PBS and filtered through a 0.22-μm filter using
: sterile technique for treatment of cells.
| R*****U
发帖数: 241 | 6 here it is for your reference:
To a three-necked flask equipped with a nitrogen source inlet, an addition
funnel and a cold thermometer, cooled to -5℃ was added a solution of methyl
glycinate hydrochloride 34 (31.7 g, 250 mmol) in water (63 mL) followed by
CH2Cl2 (150 mL). An ice-cold solution of sodium nitrite (20.9 g, 300 mmol)
in water (63 mL) was added and the reaction vessel was cooled to -10℃. An
aqueous solution of H2SO4 (5 wt%, 24 g) was added via the addition funnel
over a 3 min period. During the course of the addition, the temperature
inside the reaction flask began rise to +3℃ and the organic phase became
yellow. After the exotherm subsided (~15 min), the biphasic mixture was
poured onto ice-cold saturated aqueous sodium bicarbonate (250 mL) solution.
The layers were separated and the aqueous layer was extracted with CH2Cl2 (
30 mL). The combined organic layers were washed with cold saturated aqueous
sodium bicarbonate solution (2×250 mL) until the organic layer was no
longer acidic as indicated by litmus paper. The organic phase was washed
with water (250 mL), dried (Na2SO4), and concentrated at aspirator pressure
(23℃) to give the product 35 as a yellow oil (15.9 g, 159 mmol, 64%). The
compound was used without further purification.
IR (neat) 3122, 3002, 2957, 2113, 1704 cm-1.
1H NMR (CDCl3) δ 4.75 (s, 1H), 3.76 (s, 3H).
convert
【在 R****n 的大作中提到】
: http://www.pnas.org/content/108/8/3270.figures-only
: This is a biochem paper. The supplementary material mentioned how to convert
: a Glutamate Acid to 2-Hydroxygluataric acid. But no detailed infor
: Quote from the paper
: (R)-2-hydroxyglutarate Synthesis. (R)-2-hydroxyglutarate (2HG) was
: synthesized by treatment of D-glutamate (Sigma-Aldrich) with nitrous
: acid to forma lactone, which was then hydrolyzed with NaOH
: solution to form 2-D-hydroxylglutarate. Purity was 93%. Powder
: was resuspended in PBS and filtered through a 0.22-μm filter using
: sterile technique for treatment of cells.
| h****z
发帖数: 1996 | 7 那你想问的是什么？
methyl
by
【在 R*****U 的大作中提到】
: here it is for your reference:
: To a three-necked flask equipped with a nitrogen source inlet, an addition
: funnel and a cold thermometer, cooled to -5℃ was added a solution of methyl
: glycinate hydrochloride 34 (31.7 g, 250 mmol) in water (63 mL) followed by
: CH2Cl2 (150 mL). An ice-cold solution of sodium nitrite (20.9 g, 300 mmol)
: in water (63 mL) was added and the reaction vessel was cooled to -10℃. An
: aqueous solution of H2SO4 (5 wt%, 24 g) was added via the addition funnel
: over a 3 min period. During the course of the addition, the temperature
: inside the reaction flask began rise to +3℃ and the organic phase became
: yellow. After the exotherm subsided (~15 min), the biphasic mixture was
| R*****U
发帖数: 241 | 8 其实我原来用的很简单，就是带磨口的单口管，可以连在rotavapor上，后来我想起来
了，不过他们推荐其实很不错，比我原来的先进，
【在 h****z 的大作中提到】
: 那你想问的是什么？
:
: methyl
: by
| R****n
发帖数: 708 | 9 Looks pretty good. Thank you all! | R*****U
发帖数: 241 | 10 你的N2东西没有和酯基相连估计没有文献的稳定，不知道能像文献那样搞不？还是直接
在溶液中就反应?最好找找原始文献
哈哈
【在 R****n 的大作中提到】
: Looks pretty good. Thank you all!
| R****n
发帖数: 708 | 11 One more questions. How can I know the yield% in the end?
After crystallization, the product and the reactant may not be able to
separate.
【在 R*****U 的大作中提到】
: 你的N2东西没有和酯基相连估计没有文献的稳定，不知道能像文献那样搞不？还是直接
: 在溶液中就反应?最好找找原始文献
: 哈哈
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