Iodine → Tris(2-methoxyethoxymethyl)phosphine

関与物質

反応条件

反応手順

To ground Mg metal (5.2 g, 214 mmol) was added I2 (1 crystal), HgBr2 (10 mg) and 2 ml of a solution of 2-methoxyethoxymethyl chloride (25 g, 201 mmol) in THF (100 ml) at R.T. After 30 sec, the reaction started and was cooled to -30° C. (dry-ice/acetone). The remaining chloride/THF solution was added dropwise at -20° to -10° C. over 2 h. The mixture was stirred at 0° C. for 2h post-addition and cooled to -78° C. The reagent was then treated with PCl3 (2.2 ml, 25.1 mmol) according to General Method I and the final residue was purified by distillation to afford 1.6 (21%) of tris(2-methoxyethoxymethyl)phosphine as a colorless mobile oil (b.p.=150°-160° [email protected] mmHg). 31P-NMR(CDCl3): -42.7. MS(LREI)m/z=299(M+1 ).

情報源と証拠