تفاعل #2383771
ord-b97275aca5914982822d5965746a0bd5
معادلة التفاعل
methylene chloride
diisopropylethylamine
bis-(2-methylthioethyl)-amine
bromoacetic acid methyl ester
→
N,N-bis-(2-methylthioethyl)-glycine methyl ester
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONis added in drops under a cover-gas atmosphere
- 2غسيلwashed twice with saturated sodium bicarbonate solution
- 3تجفيفThe organic phase is dried with sodium sulfate
- 4تركيزconcentrated by evaporation
- 5أخرىthe residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol
الإجراء التجريبي
165 mg of bis-(2-methylthioethyl)-amine (Example 8b) is dissolved in 20 ml of acetonitrile and mixed with 174 μl of diisopropylethylamine. 92.7 μl of bromoacetic acid methyl ester, dissolved in 20 ml of acetonitrile, is added in drops under a cover-gas atmosphere, and the batch is stirred for 18 hours at room temperature. The acetonitrile is drawn off, the residue is taken up with methylene chloride and washed twice with saturated sodium bicarbonate solution. The organic phase is dried with sodium sulfate and concentrated by evaporation, and the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol: Yield 183 mg=77% of theory.