反応 #657261

反応方程式

trimethyl 1-trityl-3,4,5-pyrazoletricarboxylate

LiAlH4

→

1-trityl-3,4,5-tris(hydroxymethyl)pyrazole

収率 73.0%

溶媒

THF

Et2O

反応条件

後処理

1. 1
   その他After this time, the reaction was quenched by the slow addition of 1.5 mL of distilled water
2. 2
   workup.ADDITIONfollowed by addition of 1.5 mL of 10% NaOH and 3.5 mL of water
3. 3
   その他The solids formed
4. 4
   その他were removed by filtration, and 80 mL of dichloromethane
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   その他The organic phase was separated
7. 7
   洗浄washed with distilled water (70 mL)
8. 8
   その他after separation from the aqueous phase
9. 9
   乾燥was dried over MgSO4
10. 10
    その他After separation of the organic phase
11. 11
    その他the solvent was evaporated under vacuum
12. 12
    その他yielding a yellowish solid

実験手順

To a solution of trimethyl 1-trityl-3,4,5-pyrazoletricarboxylate (3.034 g, 6.26 mmol) in dry THF (60 mL) were added 50 mL of 1.0 M LiAlH4 in Et2O. The resulting solution was stirred for about 16 h at room temperature (20-25° C.). After this time, the reaction was quenched by the slow addition of 1.5 mL of distilled water, followed by addition of 1.5 mL of 10% NaOH and 3.5 mL of water. The solids formed were removed by filtration, and 80 mL of dichloromethane was added to the filtrate. The organic phase was separated, washed with distilled water (70 mL) and, after separation from the aqueous phase, was dried over MgSO4. After separation of the organic phase, the solvent was evaporated under vacuum yielding a yellowish solid. Yield: 73% (1.823 g, 4.54 mmol).

出典