関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Triphenylphosphine Oxide | HCID 13097 | — |
| 反応物 | N-Boc-Imino-(triphenyl)phosphorane | HCID 2756802 | — |
| 反応物 | 1-(5-Bromo-2-fluorophenyl)-2,2-difluoroethanone | HCID 54857833 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (Z)-tert-butyl (1-(5-bromo-2-fluorophenyl)-2,2-difluoroethylidene)carbamate | HCID 87096325 | 51.1% |
反応手順
A suspension of 1-(5-bromo-2-fluoro-phenyl)-2,2-difluoro-ethanone (16.0 g, 63.2 mmol) and N-(triphenylphosphoranylidene)-carbamic acid 1,1-dimethylethyl ester (CAS 68014-21-1) (26.3 g, 69.6 mmol) in 12 ml toluene was stirred at 100° C. for 2 days. The suspension became clear. After being cooled down somewhat, hexane was added till crystallization of triphenylphosphine oxide started. The mixture was filtered and the filtrate was purified by chromatography on silica gel with hexane/TBME 1-5% to give 11.37 g of the title compound as a yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08338413B1 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-5c131a8a8afe4d80a12fc8f74aabd2da |
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| 出典メモ | uspto-grants-2012_12 |
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