참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N,N-Dimethylglycine | HCID 673 | — |
| 반응물 | Styrene | HCID 7501 | — |
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 촉매 | Tetraphenylphosphonium Chloride | HCID 164911 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1,1-Diphenylethylene | HCID 10740 | — |
| 생성물 | trans-Stilbene | HCID 638088 | 97.4% |
| 생성물 | cis-Stilbene | HCID 5356785 | 0.6% |
반응 단계
To a reaction vessel standing on a scale which is sealed with a septum cap, 5.3 mg (0.02 mmol) of (CH3CN)2PdCl2, 45 mg (0.12 mmol) of Ph4PCl and 12.4 mg (0.12 mmol) of dimethylglycine are added, followed by two cycles of evacuation and flushing with argon. Under argon, 657.7 mg (8 mmol) of anhydrous sodium acetate and 1 ml of NMP are added. 452 mg (4.01 mmol) of Cl-benzene and 636 mg (6.11 mmol) of styrene is mixed with 1 ml of NMP and added dropwise in 6 portions within 6 hours, the first portion being added at room temperature and the others at 140° C. Stirring is performed at 140° C. for a total of 24 h. According to the processing described in Example 1 using 10 ml of diethyl ether, a 64.2% yield of Heck products (97.4% trans-stilbene, 0.6% cis-stilbene, and 2.0%- 1,1-diphenylethene) is obtained with 76.6% conversion of Cl-benzene.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06316675B1 |
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| 출처 데이터셋 | uspto-grants-2001_11 |
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| ORD ID | ord-d92d3569a6cc478798316003861e97d6 |
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| 출처 메모 | uspto-grants-2001_11 |
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