참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Butyn-1-ol | HCID 12991 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 4,6-Dichloro-5-methylpyrimidine | HCID 818860 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(2-Butynyloxy)-6-chloro-5-methylpyrimidine | HCID 22599791 | 91.2% |
반응 단계
0.32 g of sodium hydride (60% oil suspension) was suspended in 12 ml of tetrahydrofuran. 2 ml of tetrahydrofuran solution of 0.43 g of 2-butyn-1-ol was added dropwise at room temperature therein slowly, and the mixture was stirred for 20 minutes. Into the mixture was added dropwise 2 ml of tetrahydrofuran solution of 1 g of 4,6-dichloro-5-methylpyrimidine at 0° C. slowly, and stirred for 2 hours. The reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with water, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.1 g of 4-chloro-6-(2-butynyloxy)-5-methylpyrimidine.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07732448B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-527f50ac5328407d99b6df972cffea6b |
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| 출처 메모 | uspto-grants-2010_06 |
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