関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributylamine | HCID 7622 | — |
| 反応物 | 1,1,1-Trifluoro-3-phenyl-2-propanone | HCID 222958 | — |
| 反応物 | 1-(2-Amino-5-bromophenyl)-2,2,2-trifluoroethanone | HCID 46838802 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86716066 | HCID 86716066 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09309222B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-915754f82def47ea8de6a7901ec31cee |
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| 出典メモ | uspto-grants-2016_04 |
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