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CAS No. : | 172678-67-0 | MDL No. : | MFCD16036490 |
Formula : | C12H11NO2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ROKNTXACUCMRQU-UHFFFAOYSA-N |
M.W : | 233.29 | Pubchem ID : | 9899456 |
Synonyms : |
|
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 |
---|---|---|
81.8% | With sodium hydroxide; In methanol; at 20℃; for 2h; | To a solution of 1-3 (3.2 g, 13.8 mmol) in MeOH (50 mL) was added Sodium hydroxide solution (130 mL, 4 M). The reaction mixture was stirred at room temperature for 2 hours and concentrated under reduced pressure to remove MeOH. The aqueous phase was acidified with aqueous HCl (1 M) till pH=3 and the mixture was extracted with EtOAc, dried with anhydrous Na2SO4, filtered and concentrated to give the crude product. The crude product was purified by silica gel chromatography eluted to give product 1-4 (2.3 g, 81.8%). (0127) MS m/z [ESI]: 206.0 [M+1]. |
68% | With water; lithium hydroxide; In tetrahydrofuran; at 20℃; for 6h; | To a stirring solution of compound 111 (1 g, 4.28 mmol) in THF: H2O (1: 1, 20 mL) was added lithium hydroxide monohydrate (515 mg, 21.45 mmol) at room temperature and stirred for 6 h. The reaction was monitored by TLC; after completion of the reaction, the volatiles were removed in vacuo and the pH of the aqueous layer was neutralized with 1 N aqueous HCl. The precipitated solid was filtered and dried in vacuo to afford compound 112 (600 mg, 68%) as pale yellow solid. TLC: 30% EtOAc/ hexanes (Rf: 0.1); 1H NMR (DMSO-d6, 400 MHz): delta 7.93 (s, 1H), 7.92-7.88 (m, 2H), 7.51-7.43 (m, 3H); LCMS Calculated for C10H7NO2S: 205.02; LCMS observed: 206.1 (M+1)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
15% | In ethanol; | Step 20a A solution of alpha-formyl-alpha-chloroacetate (9.34 g, 49.5 mmol, 1 eq) and thiobenzamide (6.79 g, 49.5 mmol, 1 eq) in EtOH (37.0 mL) is refluxed for 1 hr. The solution changes from an orange/brown color to a deep green. This solution is washed with water and extracted with CH2Cl2. The organic fraction is dried over Na2SO4, filtered, and the solvent removed in vacuo. The product is purified by column chromatography using a Biotage Flash 40M column (20% hexanes/EtOAc) to give ethyl 2-phenyl-thiazole-5-carboxylate as a deep orange oil (1.82 g, 15%). MS (ESI) for C12H13NO3S m/z 252.1 (M+H)+. |
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