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CAS No. : | 60480-83-3 | MDL No. : | MFCD00013381 |
Formula : | C8H13ClN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ZLGXGLXFBMIVPU-UHFFFAOYSA-N |
M.W : | 172.66 | Pubchem ID : | 16213059 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
for 0.166667h;Inert atmosphere; | 10052] In 10 mL of methanol was dissolved 2,4-dimeth- ylphenylhydrazide hydrochloride (1.72 g, 10 mmol). To the solution, <strong>[186534-02-1]3,5,6-trimethylpyrazine-2-carbaldehyde</strong> (1.50 g, 12 mmol) was added with an ice-bath under the protection of N2. After the mixture was stirred for 10 mm, a lot of brick red precipitate showed and the reaction was then complete. The mixture was filtered through a suction funnel, and the brick red solid was transferred to a vacuum oven to be dried for using directly in the next reaction step of the reaction. The red brick intermediate (3.04 g, 10 mmol) was dissolved in 25 mL of methanol, and 1.68 ml of anhydrous triethylamine and 1.7 ml of trifluoroacetic anhydride were added respectively with an ice-bath under the protection of N2, and the reaction was run for 30 minutes. The reaction was monitored by TLC till completion. The resulting material was extracted with Ethyl acetate, dried over anhydrous Na2504, separated by a silica gel colunm (ethyl acetate:petroleum ether=1 :3) to get T-006 as a light yellow solid (3.25 g, 89.3%). ESI-MS: [M+H] mlz 365.1. ?H-NMR (CDC13, 300 MHz) oe: 2.1 (s, 3H), 2.42 (s, 3H), 2.46 (s, 3H), 2.54 (s, 3H), 2.85 (s, 3H), 7.08 (d, j=7.05 Hz, 1H), 7.24 (d, J=7.21 Hz, 1H), 7.25 (s, 1H), 7.55 (s, 1H); Anal. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; for 0.166667h;Cooling with ice; Inert atmosphere; | In 10 mL of methanol was dissolved 2,4-dimethylphenylhydrazide hydrochloride (1.72 g, 10 mmol). To the solution, <strong>[186534-02-1]3,5,6-trimethylpyrazine-2-carbaldehyde</strong> (1.50 g, 12 mmol) was added with an ice-bath under the protection of N2. After the mixture was stirred for 10 min, a lot of brick red precipitate showed and the reaction was then complete. The mixture was filtered through a suction funnel, and the brick red solid was transferred to a vacuum oven to be dried for using directly in the next reaction step of the reaction. The red brick intermediate (3.04 g, 10 mmol) was dissolved in 25 mL of methanol, and 1.68 ml of anhydrous triethylamine and 1.7 ml of trifluoroacetic anhydride were added respectively with an ice-bath under the protection of N2, and the reaction was run for 30 minutes. The reaction was monitored by TLC till completion. The resulting material was extracted with Ethyl acetate, dried over anhydrous Na2SO4, separated by a silica gel column (ethyl acetate:petroleum ether=1: 3) to get T-006 as a light yellow solid (3.25 g, 89.3%). ESI-MS: [M+H]+ m/z 365.1. 1H-NMR (CDCl3, 300 MHz) delta: 2.1 (s, 3H), 2.42 (s, 3H), 2.46 (s, 3H), 2.54 (s, 3H), 2.85 (s, 3H), 7.08 (d, j=7.05 Hz, 1H), 7.24 (d, J=7.21 Hz, 1H), 7.25 (s, 1H), 7.55 (s, 1H); Anal. (C18H19F3N4O) C, H, C; found C, 59.44%, H, 5.319%, N, 15.23%; requires: C, 59.33%, H, 5.26%, N, 15.38%. |
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