참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Cyanide | HCID 8929 | — |
| 반응물 | 2-(Chloromethyl)-4,6-dimethoxypyrimidine | HCID 10965279 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 2-(4,6-Dimethoxypyrimidine-2-yl)acetonitrile | HCID 14580674 | 58% |
반응 단계
16.7 g of dried sodium cyanide are dissolved in 850 ml of dimethyl sulfoxide at 90° C. under N2 protective gas. At this temperature, 52.8 g of 2-chloromethyl-4,6-dimethoxypyrimidine, dissolved in 280 ml of dimethyl sulfoxide, are added dropwise over the course of 2 hours. Stirring is continued for 1 hour at 90° C., and the mixture is cooled to room temperature and poured into 300 ml of water. The aqueous phase is extracted seven times using ether, and the combined organic phases are washed using saturated aqueous sodium chloride solution, dried over magnesium sulfate and evaporated in a rotary evaporator. This gives 29.1 g of crude product, from which 2-cyanomethyl-4,6-dimethoxypyrimidine of melting point 65°-67° C. are obtained after column chromatography (SiO2 ; CH2Cl2 /CH3OH; 98.5/1.5).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05053072 |
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| 출처 데이터셋 | uspto-grants-1991_10 |
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| ORD ID | ord-3e2838a069f84763940e5d1b25a2f2c0 |
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| 출처 메모 | uspto-grants-1991_10 |
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