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3-bromopropylamine hydrobromide

triphenylphosphine

→

title compound

수율 117.3%

(3-aminopropyl)(triphenyl)phosphonium dibromide

수율 117.3%

용매

1-butanol

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후처리

1. 1
   기타The solution was degassed again
2. 2
   기타by bubbling nitrogen through it for 10 minutes
3. 3
   온도The solution was cooled
4. 4
   workup.ADDITIONpoured into a stirring solution of methyl t-butyl ether (700 mL) and toluene (400 mL)
5. 5
   기타resulted
6. 6
   여과the solids were filtered
7. 7
   세척the product cake rinsed two times with methyl t-butyl ether (2×100 mL)

실험 절차

To a stirred, degassed solution of 3-bromopropylamine hydrobromide (25.1 g, 115 mmol) in 1-butanol (210 mL) was added triphenylphosphine (42.1 g, 160 mmol). The solution was degassed again by bubbling nitrogen through it for 10 minutes and then heated at 120° C. overnight. The solution was cooled and poured into a stirring solution of methyl t-butyl ether (700 mL) and toluene (400 mL). After stirring at room temperature until a homogenous slurry resulted, the solids were filtered and the product cake rinsed two times with methyl t-butyl ether (2×100 mL) to afford the title compound (54 g, 84%), as a white solid.

출처