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HRID 47969作成日:2026年10月26日

Methanol → 8-(3-{[Bis(methylethyl)amino](2-cyanoethoxy)phosphinooxy}propyl)-7-oxophenoxazin-3-yl 2,2-dimethylpropanoate

https://huagongshe.com/reaction/47969

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物TriethylamineHCID 8471—
反応物2-Cyanoethyl N,N-diisopropylchlorophosphoramiditeHCID 2734844—
反応物8-(3-Hydroxypropyl)-7-oxophenoxazin-3-yl 2,2-dimethylpropanoateHCID 22672525—
溶媒Diethyl EtherHCID 3283—
溶媒DichloromethaneHCID 6344—
溶媒HexaneHCID 8058—
生成物8-(3-{[Bis(methylethyl)amino](2-cyanoethoxy)phosphinooxy}propyl)-7-oxophenoxazin-3-yl 2,2-dimethylpropanoateHCID 22672527—

反応手順

36b (0.38 g, 1.1 mmol) was dissolved in 6 mL of anhydrous CH2Cl2. Triethylamine (1.5 mL) was added followed by 2-cyanoethyl diisopropylchlorophosphoramidite (0.29 mL, 1.3 mmol). The solution was kept at room temperature for 30 min, MeOH (0.1 mL) was added and the reaction was concentrated under vacuum. The residue obtained was partitioned between ethyl acetate and NaHCO3. The organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated to afford the crude amidite. It was dissolved in 2 mL of ether and added dropwise to ˜50 mL of hexane. The resultant orange solid was collected by filtration, washed with hexane and dried. The yield was 0.4 g.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06699975B2
出典データセットuspto-grants-2004_03
ORD IDord-12f83a610c1f470193d59c21eab882af
出典メモuspto-grants-2004_03