참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 1-Iodo-4-nitrobenzene | HCID 12495 | — |
| 반응물 | methylphosphonoylmethane | HCID 178503022 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | (1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium | HCID 6505921 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-(Dimethyl-phosphinoyl)-4-nitro-benzene | HCID 21897912 | 36.3% |
반응 단계
A degassed suspension of 1-iodo-4-nitrobenzene (90 mg, 0.36 mmol), dimethylphosphane oxide (29.2 mg, 0.38 mmol), bis(dibenzylideneacetone)palladium (3.31 mg, 0.0036 mmol), XantPhos (6.27 mg, 0.0108 mmol), and Cs2CO3 (165 mg, 0.506 mmol) in dry dioxane (0.4 mL) was heated in a sealed tube at 90° C. for 4 h. The cooled mixture was filtered, the filtrate concentrated in vacuo, and the residue chromatographed over silica gel eluting with 5% MeOH in dichloromethane to afford 26 mg of dimethyl(4-nitrophenyl)phosphane oxide (yield: 36%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09096624B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-888e2891d838492ab0fee53c43e5e966 |
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| 출처 메모 | uspto-grants-2015_08 |
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