참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 3-Pentyn-2-ol | HCID 141344 | — |
| 반응물 | 4-Chloro-6-(2,6-difluorobenzyl)pyrimidine | HCID 22599701 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(2,6-Difluorobenzyl)-6-(1-methyl-2-butynyloxy)pyrimidine | HCID 22599865 | 133.6% |
반응 단계
In 1 ml of tetrahydrofuran was suspended 0.04 g of sodium hydride (60% in oil), to which 0.2 ml of a tetrahydrofuran solution containing 0.06 g of 3-pentyn-2-ol was slowly added dropwise under stirring at room temperature. The mixture was stirred at room temperature for 20 minutes, and 0.4 ml of a tetrahydrofuran solution containing 0.15 g of 4-chloro-6-(2,6-difluorobenzyl)pyrimidine was slowly added dropwise at room temperature, followed by stirring for 3 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution and extracted three times with ethyl acetate. The organic layers were combined, washed with water, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.24 g of 4-(2,6-difluorobenzyl)-6-(1-methyl-2-butynyloxy)pyrimidine (the present compound (147)).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06838463B2 |
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| 출처 데이터셋 | uspto-grants-2005_01 |
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| ORD ID | ord-e5a2ccc2f25b4cafb5502ee2c4563a42 |
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| 출처 메모 | uspto-grants-2005_01 |
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