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HRID 253047作成日:2026年10月26日

Triethylamine → HCID 15462093、化合物

https://huagongshe.com/reaction/253047

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物3-Chloro-6-phenylpyridazineHCID 88515—
反応物(1S,4S)-2-Boc-2,5-diazabicyclo[2.2.1]heptaneHCID 11521263—
溶媒TolueneHCID 1140—
生成物HCID 15462093HCID 1546209349.2%

反応条件

温度100 °C

反応手順

Triethylamine (20 mL) was added to a suspension of t-butyl (S,S)-2,5-diazabicyclo[2.2.1]heptane-2-carboxylate (3.43 g, 17.3 mmol, Aldrich Chemical Company) and 3-chloro-6-phenylpyridazine (3.30 g, 17.3 mmol, Aldrich Chemical Company) in toluene (50 mL) and the mixture was heated under nitrogen at 100° C. for 7 days. The dark mixture was cooled to room temperature, and the resulting precipitate was isolated by filtration, washed with toluene (15 mL) and dried under vacuum to provide the title compound as an off-white solid (3.00 g). The filtrate was concentrated and the residue wa purified by column chromatography on silica gel, eluting with ethyl acetate, to provide additional product (0.41 g, total yield 3.41 g, 56%): MS (DCI/NH3) m/z 353 (M+H)+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07872017B2
出典データセットuspto-grants-2011_01
ORD IDord-14be6efbf7eb448b9aad427d153e60f1
出典メモuspto-grants-2011_01