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HRID 233649作成日:2026年10月27日

Water → 3beta-(2-(N-(2-(1-Pyrrolidinyl)ethyl)methylamino)ethylthio)-17beta-(3-furyl)-5beta-androstan-14beta-ol

https://huagongshe.com/reaction/233649

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium hydrideHCID 24758—
反応物Methyl(2-(pyrrolidin-1-yl)ethyl)amineHCID 295976—
反応物3beta-(2-Tosyioxyethylthio)-17beta-(3-furyl)-5beta-androstan-14beta-olHCID 86748785—
溶媒DimethylformamideHCID 6228—
生成物3beta-(2-(N-(2-(1-Pyrrolidinyl)ethyl)methylamino)ethylthio)-17beta-(3-furyl)-5beta-androstan-14beta-olHCID 7004602760.7%

反応手順

To a solution of 0.34 g of N-(2-(1-pyrrolidinyl)ethyl)methylamine in 5 ml of dimethylformamide, 0.045 g of NaH (60% dispersion in mineral oil) were added under nitrogen and the mixture was stirred at room temperature for half an hr; a solution of 0.50 g of 3β-(2-tosyloxyethylthio)-17β-(3-furyl)-5β-androstan-14β-ol, prepared as described in Ex. 51, in 2 ml of dimethylformamide was added, the mixture was stirred for another 4 hrs and then 7 ml of water were poured in. The residue was extracted with ethyl acetate, the organic solution was washed with water to neutral pH, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The crude product was purified by flash-chromatography (SiO2) using methylene chloride/methanol 95/5 as eluant to give 0.28 g of the title compound (I-ca) as an amorphous solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05593982
出典データセットuspto-grants-1997_01
ORD IDord-02c04493e8584137a08185b56d60bf2e
出典メモuspto-grants-1997_01