反応 #160830

反応方程式

diphenylphosphinic chloride

( 2 )

diamide

hydroxylamine-HCl

NaOH

→

above compound

収率 82.5%

(aminooxy)(diphenyl)phosphine oxide

収率 82.5%

溶媒

—

ice

dioxane

water

water

dioxane

反応条件

後処理

1. 1
   その他A 5 L 4-neck round bottom flask (rbf) fitted with an overhead stirrer
2. 2
   workup.ADDITIONa thermocouple was charged with
3. 3
   workup.ADDITIONadded all at once)
4. 4
   その他rose to 22° C
5. 5
   ろ過filtered
6. 6
   workup.WAITThe crude material was left on the frit
7. 7
   workup.WAITto drain for one hour
8. 8
   workup.STIRRINGvigorously stirred for five minutes (no more than 10 min)
9. 9
   ろ過filtered again
10. 10
    洗浄washing 2× with ice cold water
11. 11
    workup.WAITleft
12. 12
    その他to dry overnight on the fritted filter
13. 13
    その他The partially dried material was dried for 12 h in a vacuum oven (50° C., 0.1 torr)
14. 14
    その他well crushed with a mortar & pestal
15. 15
    その他An additional 16 h of drying in the vacuum oven

実験手順

A 5 L 4-neck round bottom flask (rbf) fitted with an overhead stirrer & a thermocouple was charged with; (1) a solution of NaOH (60.85 g, 1.52 mol, 2.4 eq) in 180 mL water, (2) a solution of hydroxylamine-HCl (110.12 g, 1.58 mol, 2.5 eq) in 180 mL water and (3) 180 mL dioxane. The mixture was cooled in an ice/acetone bath to 0° C. 150 g of ice was added, followed by a precooled (to about 10° C.) solution of diphenylphosphinic chloride (150.0 g, 0.634 mol, 1 eq) in 180 mL dioxane (added all at once). The reaction became very thick with a white precipitate, requiring vigorous stirring. The internal temperature rose to 22° C. After 5 additional minutes stirring (10 minutes maximum), the reaction mixture was diluted with 2.5 L of ice cold water and filtered thru a large fritted funnel (15 cm diameter). The crude material was left on the frit to drain for one hour, then transferred back into the 5 L rbf. The solid was suspended in 500 mL ice cold 0.25N NaOH solution and vigorously stirred for five minutes (no more than 10 min), then filtered again, washing 2× with ice cold water and left to dry overnight on the fritted filter. The partially dried material was dried for 12 h in a vacuum oven (50° C., 0.1 torr) and then well crushed with a mortar & pestal. An additional 16 h of drying in the vacuum oven afforded 122 g (82%) the above compound as a white powder.

出典