참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Phosphorus pentachloride | HCID 24819 | — |
| 반응물 | 6-Hydroxymethyl-N,N-dicyclopentylnicotinamide | HCID 20071644 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 6-Chloromethyl-N,N-dicyclopentylnicotinamide | HCID 20071639 | — |
반응 단계
To a solution of the title product of Example C (1.44 g, 5 mmol) in chloroform (30 mL), phosphorus pentachloride (1.04, 5 mmol) was added. The contents were immersed in an oil-bath at 70° C. and the temperature raised to reflux. After 18h, the pinkish colored reaction solution was cooled to room temperature. The reaction was diluted with water (75 mL) and solid potassium carbonate (2.2 g) added. The contents were stirred for about 10 min until no more effervescence was observed. More water (100 mL) was added and the reaction solution extracted with methylene chloride. The organic layer was separated, dried (MgSO4) and filtered. After removal of solvent, 1 6 g of the title product was isolated as an off-white solid. The compound was used in Example 1 without any further purification. 1H NMR (CDCl3) 1,2-2.2 (m, 16H), 3.6-3.9 (m, 2H), 4.7 (s, 2H), 7.53 (d,J=8 Hz, 1H), 7.74 (dd,J=3,8 Hz, 1H), and 8.56 ppm (d,J=3 Hz, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04990518 |
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| 출처 데이터셋 | uspto-grants-1991_02 |
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| ORD ID | ord-a693ee75bc374c9ba8ef06ca95f86424 |
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| 출처 메모 | uspto-grants-1991_02 |
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