6-溴-2-氨甲基吡啶的合成？ < >我需要合成一个中间体：6-溴-2-氨 甲基吡啶 ，查了好多，竟没有好的文献报道，只一篇专利，利用2-羟甲基-6-溴吡啶，邻 苯二甲酰亚胺 ，三苯基磷，及 偶氮二甲酰二哌啶 ，用一锅煮法，在跟踪发现，大部分原料没办法反应，请高手提点建议，谢谢。</P> < >附：专利原文</P> < align=left>Example 210 Preparation <RTI>of N-r6-92-(2, 4-Dichloro-benzovl)-3-methyl-benzofuran-6-yll-Pvridin-2- </RTI><RTI>vlmethyl-acetamide</RTI> <DP N="91" /><EMI><EMI><TXF HE="5" WI="130" LX="425" LY="742" FR="1" FONT="Times" SIZE="10" LS="59" />Step 1: Preparation <RTI>of 6-2- (6-Bromo-pvridin-2-vlmethvl)-isoindole-1, </RTI>3-dione <EMI><TXF HE="122" WI="3" LX="151" LY="1200" FR="2" FONT="Times" SIZE="9" LS="1676" />< LN N="5" />< LN N="10" />< LN N="15" />< LN N="20" /><TXF HE="71" WI="152" LX="294" LY="1129" FR="3" FONT="Times" SIZE="12" LS="330" />(6-Bromo-pyridin-2-yl)-methanol (2949 mg, 15.68 <RTI>mmol),</RTI> phthalimide (3000mg, 20.39 <RTI>mmol),</RTI> triphenylphosphine (5348 mg, 20.39 <RTI>mmol)</RTI> and 1, <RTI>1- (azodicarbonyl)- </RTI>dipiperidine) 5144,20. 39 <RTI>mmol)</RTI> were dissolved in THF (150 mL) and stirred at room temperature for 4h. The reaction mixture was cooled to <RTI>0°C</RTI> and the resulting precipitate was removed via filtration. A saturated aqueous sodium bicarbonate solution was added to the filtrate and the solution was extracted several times with ethyl acetate. The combined organic extracts were dried over magnesium sulfate and condensed under reduced pressure. The crude residue was purified by column chromatography with a gradient of 10 to 75% <RTI>AcOEt/hexanes</RTI> to give 2- (6-Bromo-pyridin-2-ylmethyl)-isoindole- 1,3-dione as a white solid (4000 mg, 80 %) MS ES (MH+ 317.2/319. 1). </P> < align=left>Step 2 Preparation of <RTI>C-(6-Bromo-pyridin-2-vl)-methvlamine</RTI> <EMI><TXF HE="52" WI="153" LX="291" LY="2100" FR="4" FONT="Times" SIZE="12" LS="169" />A suspension of <RTI>2- (6-Bromo-pyridin-2-ylmethyl)-isoindole-1, </RTI>3-dione (4000 mg, 12.61 <RTI>mmol)</RTI> in ethanol (60 mL) was heated at <RTI>70°C</RTI> until complete dissolution was observed. </P> < align=left>Hydrazine hydrate (3156 mg, 63.06 <RTI>mmol)</RTI> was then added and the resulting mixture was heated at <RTI>70°C</RTI> for 5h. The resulting solution was cooled to <RTI>0°C</RTI> and filtered. The filtrate was concentrated in vacuo and the crude residue was purified by column chromatography with a gradient of 0 to 30% <RTI>methanol/dichloromethane</RTI> to give <RTI>C- (6- </RTI>Bromo-pyridin-2-yl)-methylamine as a yellow solid (2070 mg, 79%). MS ES (MH+ 187.1, <RTI>RT = </RTI>1. 11 min). <DP N="92" /><EMI><TXF HE="5" WI="110" LX="420" LY="254" FR="1" FONT="Times" SIZE="10" LS="59" /></P>查看更多6个回答 . 4人已关注
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