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Tris(2-carboxyethyl)phosphine hydrochloride (TCEP ) (7.0 g, 24.42 mmol) was co- evaporated with EtOH (2 x 100 ml), dissolved in CH3OH (200 ml) at 4 °C, and then thionyl chloride (9.0 ml ., 122.29 mmol) was added. The resulting mixture was stirred for at RT overnight, concentrated, and dried over vacuum to provide the title compound (7.0 g, 98percent yield), ESI MS m//+ 293.2 (M + H).
Tris(2-carboxyethyl)phosphine hydrochloride (TCEP ) (7.0 g, 24.42 mmol) was co- evaporated with EtOH (2 x 100 ml), dissolved in CH3OH (200 ml) at 4 C, and then thionyl chloride (9.0 ml ., 122.29 mmol) was added. The resulting mixture was stirred for at RT overnight, concentrated, and dried over vacuum to provide the title compound (7.0 g, 98% yield), ESI MS m//+ 293.2 (M + H).
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃; for 4.0h;
Trimethyl 3,33''-phosphinetriyltripropanoate (7.0 g, 23.96 mmol) in I I II (100 ml) at 0 C was added L1AIH4 (2 M) in I I II (70ml). The reaction was stirred for 4 h at 0 C, quenched with cold water (5 ml), filtered, evaporated to dryness to afford crude 3,3',3"~ phosphinetriyltris (propan-l-ol) (5.1 g, 102% yield) which was used directly for next step. This compound dissolved in HOAc (80 ml) was added I ? ? (20 ml, 33% in water). The mixture was stirred for overnight, concentrated, co-evaporated with water (2 x 100 ml) and toluene, and dried over vacuum to afford the title compound (4.88 g, 91 % yield).