참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Felbinac | HCID 3332 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Diethyl cyanophosphonate | HCID 76257 | — |
| 반응물 | 3,4-Bis(benzyloxy)phenethylamine hydrochloride | HCID 423869 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-biphenyl-4-yl-N-[2-(3,4-bis-benzyloxy-phenyl)-ethyl]-acetamide | HCID 11785829 | — |
반응 단계
The intermediate 2-biphenyl-4-yl-N-[2-(3,4-bis-benzyloxy-phenyl)-ethyl]-acetamide (1) was prepared as follows: To a stirred solution of 2.85 g (7.7 mmol) of 3,4-dibenzyloxyphenethyl amine and 1.49 g (7 mmol) of 4-biphenylacetic acid in 20 ml of anhydrous dimethylformamide at 0° C., 2.5 ml (17.7 mmoles) of triethyl amine was added dropwise and then 1.4 ml (7.7 mmol) of diethyl cyanophosphonate (90% purity) was added dropwise. The reaction mixture was stirred for 22 hours and allowed to reach room temperature, and then it was poured into 300 ml of water. The precipitated solid was separated on a glass filter funnel, washed with water (3×70 ml), and air-dried overnight. This solid was recrystallized using hexanes/ethanol mixture to provide 3.1 g (84%) of grayish crystals, mp 142-144° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07241774B2 |
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| 출처 데이터셋 | uspto-grants-2007_07 |
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| ORD ID | ord-72fecbe6f4f947fca934c4a2d43b98e3 |
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| 출처 메모 | uspto-grants-2007_07 |
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