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HRID 627477作成日:2026年10月25日

Tributylamine → HCID 86716066、化合物

https://huagongshe.com/reaction/627477

反応式

関与物質

役割名称HCID仕込み量
反応物TributylamineHCID 7622—
反応物1,1,1-Trifluoro-3-phenyl-2-propanoneHCID 222958—
反応物1-(2-Amino-5-bromophenyl)-2,2,2-trifluoroethanoneHCID 46838802—
溶媒DimethylformamideHCID 6228—
生成物HCID 86716066HCID 86716066—

反応条件

温度130 °C

反応手順

A yellow solution of 1-(2-amino-5-bromophenyl)-2,2,2-trifluoroethanone (1.32 g, 4.94 mmol, Intermediate 8, step b) and 1,1,1-trifluoro-3-phenylpropan-2-one (0.980 g, 5.21 mmol) in DMF (4.95 mL) was treated with tributylamine (1.23 mL, 5.19 mmol) and stirred at 130° C. under air (capped) for 2 hours. The homogeneous orange solution was then cooled to room temperature and partitioned with ether (8 mL) and 1 M NaH2PO4 (8 mL). The organic layer was washed with 1 M NaH2PO4 (1×8 mL), dried (Na2SO4), filtered, and concentrated, and the residue was flash chromatographed with a heptane to 30% DCM/heptane gradient to yield the title compound as a nearly colorless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09309222B2
出典データセットuspto-grants-2016_04
ORD IDord-915754f82def47ea8de6a7901ec31cee
出典メモuspto-grants-2016_04