Efforts to prepare the desired sila

Efforts to prepare the desired silane directly via amidation of
triethylphosphonoacetate (1a) with aminopropyltriethoxysilane
(2) were unsuccessful (the reaction required elevated tem￾peratures and generated multiple side products).
Thus, our focus turned to the trifluoroethyl analog (1b). This
material was prepared in straightforward fashion by treating
diethylphosphonoacetic acid with thionyl chloride, and subse￾quently with trifluoroethanol.5 After distillation, the desired
trifluoroethyl ester was obtained in 58% yield.6 Exposure of 1b
to neat 2, resulted in a moderate exotherm and the clean
production of the desired CMPO silane (3).7 Attempts to purify
3 via vacuum distillation resulted in partial decomposition of
the product. Fortunately, the reaction affording 3 is sufficiently
clean as to allow direct usage of the crude product (we simply
removed the trifluoroethanol by-product under vacuum).

結果 (中文) 1:

准备所需的硅烷直接通过酰胺化的努力triethylphosphonoacetate (1a) 与法（2） 都不成功，（所需的反应温度升高和生成多个侧产品）。因此，我们关注的焦点转向三氟乙基模拟 (1b)。这制得的材料是以简单的方式治疗二乙基磷乙酸氯化亚砜，与实验结果表明灾民与经过蒸馏、 所需的 trifluoroethanol.5三氟乙基酯制得在 58%yield.6 1b 曝光到整洁 2，导致温和放热和清洁生产所需 CMPO 硅烷 (3).7 试图净化3 通过真空蒸馏导致部分分解该产品。幸运的是，给予 3 的反应是足够清洁并允许直接使用粗品的 (我们只是删除在真空下的乙醇副产品）。

結果 (中文) 3:

经酰胺化制备所需的硅烷直接努力triethylphosphonoacetate（1A）与氨丙基三乙氧基硅烷（2）是不成功的（反应所需的温度升高的TEM￾并产生多个副产品）。因此，我们的重点转向了三氟模拟（1B）。这以简单的方式处理材料diethylphosphonoacetic酸与氯化亚砜，以及后续的￾频繁与三氟乙醇5蒸馏后，所需。在58%的收益率获得了三氟乙酯。1B曝光6整齐的2，导致在一个温和的放热和清洁所需的CMPO硅烷的生产（3）7次净化。3通过真空蒸馏导致部分分解产品。幸运的是，3的反应提供足够清洁，以允许直接使用的原油产品（我们简单地三氟乙醇副产品在真空下除去）。