참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Bromoanisole | HCID 7730 | — |
| 반응물 | Phenylphosphonic dichloride | HCID 69990 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 촉매 | 1,2-Dibromoethane | HCID 7839 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Bis(4-methoxyphenyl)phenylphosphine oxide | HCID 4589182 | 93% |
반응 단계
A slurry of magnesium (133.7 g, 5.50 mol), tetrahydrofuran (988 g), and 1,2-dibromoethane (0.1 g, 0.5 mmol) was refluxed for 20 min. under a blanket of nitrogen. 4-Bromoanisole (1002 g, 5.357 mol) was added by drop over 6 h at a rate to maintain 70° C. The reaction mixture was heated for an additional hour. Dichlorophenylphosphine oxide (479.4 g, 2.459 mol) was added by drop to maintain a temperature of 35° C. over 5 h. The reaction mixture was worked up to give bis(4-methoxyphenyl)phenylphosphine oxide (770.8 g, 93% yield) as a viscous amber oil. 31P NMR: (d6-DMSO) δ 30.2 (s).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06955851B2 |
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| 출처 데이터셋 | uspto-grants-2005_10 |
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| ORD ID | ord-7bdb4826e01942ac9a6045b74fe87bf9 |
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| 출처 메모 | uspto-grants-2005_10 |
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