関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Bromo-3-phenyl-6-(3-phenylpropoxy)indene-1-one | HCID 68695076 | — |
| 触媒 | Copper(1+) | HCID 104815 | — |
| 生成物 | 1-oxo-3-phenyl-6-(3-phenylpropoxy)-1H-indene-2-carbonitrile | HCID 68695089 | 80% |
反応手順
2-Bromo-3-phenyl-6-(3-phenyl-propoxy)-indene-1-one (1.0 g, 2.3 mmol) obtained in Step 2 was dissolved in N,N-dimethyl formamide (10 mL), copper(I) cyamide (617 mg, 6.9 mmol) was added thereto, and the mixture was stirred for 3 hrs at 150° C., followed by cooling. The resulting mixture was washed with saturated ammonium chloride and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography (ethyl acetate:hexane=1:3) to obtain 700 mg of the titled compound (yield: 80%) as a red solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745439B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-25ef1506204e440cafabec79ffa9cfc6 |
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| 出典メモ | uspto-grants-2010_06 |
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