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HRID 471018作成日:2026年10月26日

Triethylamine → (9-(3-(2-Hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-isopropylthiazol-4-yl)methanone

https://huagongshe.com/reaction/471018

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物Benzeneethanol, 3-(bromomethyl)-HCID 18999576—
反応物(2-Isopropylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetateHCID 66964182—
溶媒AcetonitrileHCID 6342—
生成物(9-(3-(2-Hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-isopropylthiazol-4-yl)methanoneHCID 57989126—

反応手順

A mixture of (2-isopropylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate (example 22, step b) (0.85 g) and 2-(3-(bromomethyl)phenyl)ethanol (example 6, step a) (0.432 g) in acetonitrile (10 mL) at 20° C. was treated with triethylamine (0.616 mL) and then stirred for 2 hours. The solvent was evaporated under reduced pressure and the residue partitioned between ethyl acetate and brine, the organic layer was dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography, elution gradient 1% triethylamine and 3% methanol in dichloromethane. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.71 g.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08629271B2
出典データセットuspto-grants-2014_01
ORD IDord-fb021460c82947818441a48d72c0549c
出典メモuspto-grants-2014_01