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CAS No. : | 16652-76-9 | MDL No. : | MFCD00038908 |
Formula : | C19H25NO5S | Boiling Point : | - |
Linear Structure Formula : | C12H17NO2·C7H8SO3 | InChI Key : | QWUQVUDPBXFOKF-MERQFXBCSA-N |
M.W : | 379.47 | Pubchem ID : | 11567066 |
Synonyms : |
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Chemical Name : | H-Val-Obzl.TosOH |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine; In toluene; for 1h;Heating / reflux;Product distribution / selectivity; | A mixture of L-Valine benzyl ester tosylate (132.7 g), 4-(5,5-dimethyl- [1 ,3,2]dioxaborinan-2-yl)-benzaldehyde (330 ml_), Et3N (48.4 ml_) and toluene (413 ml_) was heated at reflux temperature for 1 h. The water while formed was azeotropically separated. Then, the mixture was cooled to room temperature and the solution was washed with aqueous NaHCO3 (317 ml_ x 2) and water (317 ml_). The residual water was azeotropically removed. The toluene was partially distilled (134 ml_) and MeOH (134 ml_) was added. The solution was then cooled to 0-5 0C and NaBH4 (6.5 g) was slowly added. The reaction mixture was stirred at room temperature overnight. Then the solvent was partially distilled (half volume) and the residue was washed with aqueous NaHCO3 (270 ml_). The separated aqueous phase was extracted with toluene (135 ml_ x 2). The combined organic phases were then washed with water (135 ml_). The residual water in the organic layer was azeotropically removed and the residue (aprox. 730 ml_) was used directly in the next step. 1H-NMR (400 MHz, CDCI3): delta 0.91 and 1.02 (s and m, 12 H, CH3), 1.77 (bs, 1 H, NH), 1.93 (m, 1 H, CH(CH3)2), 1.82 (bs, 1 H, NH), 3.05 (d, 1 H, J = 6.4 Hz, CH-N), EPO <DP n="18"/>3.58 and 3.83 (2 d, J = 13.2 Hz, 1 H each, CH2-Ph), 5.16 (s, 2 H, CH2-Ph), 7.28 (d, 2 H, J = 8 Hz, H-Ar), 7.36 (bs, 5 H, H-Ar), 7.73 (d, 2 H, J = 8 Hz, H- Ar) ppm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example 3: Preparation of (benzyl N-r4-(5,5-dimethyl-H ,3,21dioxaborinan-2- yl)phenyl-4-yl-methyll-L-valinate); A mixture of L-Valine benzyl ester tosylate (132.7 g), 4-(5,5-dimethyl- <n="19"/>[1 ,3,2]dioxaborinan-2-yl)-benzaldehyde (330 ml_), Et3N (48.4 mL) and toluene (413 mL) was heated at reflux temperature for 1 h. The water while formed was azeotropically separated. Then, the mixture was cooled to room temperature and the solution was washed with aqueous NaHCO3 (317 mL x 2) and water (317 mL). The residual water was azeotropically removed. The toluene was partially distilled (134 mL) and MeOH (134 mL) was added. The solution was then cooled to 0-5 0C and NaBH4 (6.5 g) was slowly added. The reaction mixture was stirred at room temperature overnight. Then the solvent was partially distilled (half volume) and the residue was washed with aqueous NaHCO3 (270 mL). The separated aqueous phase was extracted with toluene (135 mL x 2). The combined organic phases were then washed with water (135 mL). The residual water in the organic layer was azeotropically removed and the residue (aprox. 730 mL) was used directly in the next step. |