참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Triphenylphosphine Oxide | HCID 13097 | — |
| 반응물 | N-Boc-Imino-(triphenyl)phosphorane | HCID 2756802 | — |
| 반응물 | 1-(5-Bromo-2-fluorophenyl)-2,2-difluoroethanone | HCID 54857833 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | (Z)-tert-butyl (1-(5-bromo-2-fluorophenyl)-2,2-difluoroethylidene)carbamate | HCID 87096325 | 51.1% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08846658B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-bd1ac46e42b9420bae8c3dd10c663828 |
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| 출처 메모 | uspto-grants-2014_09 |
|---|
