反応 #2374017

反応方程式

potassium

naphthalene

→

potassium naphthalene

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度The solution was then warmed to -80° C.
2. 2
   workup.STIRRINGstirred for 18 hours at this temperature
3. 3
   温度slowly warmed to room temperature
4. 4
   ろ過The resultant solution was filtered
5. 5
   その他evaporated to dryness
6. 6
   その他giving a dark brown solid
7. 7
   その他The latter gave
8. 8
   その他a broad metal-hydride absorption band in the infrared region at 1800 cm-1

実験手順

A solution of potassium naphthalene was prepared from potassium (110 mg) and naphthalene (400 mg), in tetrahydrofuran (40 ml). This was added to a suspension of [(Ph2CH3P)2RuCl]2H (780 mg) in 40 ml of tetrahydrofuran, cooled to -111° C. The reducing metal arene solution was added slowly, and the reaction mixture, at -111° C. was vigorously agitated throughout the addition. The solution was then warmed to -80° C., and stirred for 18 hours at this temperature, then slowly warmed to room temperature. The resultant solution was filtered and evaporated to dryness giving a dark brown solid. The latter gave a broad metal-hydride absorption band in the infrared region at 1800 cm-1. On the basis of the elemental analyses of this crude product, we regard the composition as being [(Ph2CH3P)3RuH]-K+.

出典