참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | (2-Chloropyridin-4-yl)methanol | HCID 7062237 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (2-Chloropyridin-4-yl)methyl methanesulfonate | HCID 53436764 | 107.2% |
반응 단계
To a 0° C. solution of (2-chloro-pyridin-4-yl)-methanol (2.00 g, 13 mmol) (prepared from the corresponding carboxylic acid according to the procedure in U.S. Pat. No. 6,218,537), ethyl acetate (30 mL) and triethylamine (2.9 mL, 21 mmol) was added drop wise methansulfonyl chloride (1.4 mL, 18 mmol). The solution was stirred for 10 minutes and then water (5 mL) was added. The reaction mixture was extracted with three 30 mL portions of ethyl acetate, the organics combined and washed with water (30 mL) and brine (30 mL), dried on sodium sulfate, and concentrated to a crude oil. Pentane was added to the residue and stirred at 0° C. The precipitate was collected and dried in vacuo to give methanesulfonic acid 2-chloro-pyridin-4-ylmethyl ester (3.09 g, 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06759428B2 |
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| 출처 데이터셋 | uspto-grants-2004_07 |
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| ORD ID | ord-31704c4e0c9d4be997a6005f79446e78 |
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| 출처 메모 | uspto-grants-2004_07 |
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