참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | 2,6-Bis(chloromethyloxy-carbonyloxymethyl)pyridine | HCID 14749555 | — |
| 생성물 | 2,6-bis(hydroxymethyl)pyridine bis(N-methylcarbamate) | HCID 23615944 | 97% |
반응 단계
3.15 ml of methanolic methylamine solution (containing 33.6% by weight, i.e. 0.024 moles, of methylamine) are added to a solution of 1.3 g (0.004 moles) of 2,6-bis(chloromethyloxy-carbonyloxymethyl)pyridine (prepared as described in Example 1) at about 0° C. under cooling at such a rate that the temperature is maintained at 10° C. or lower. A crystalline precipitate is separated. After completing the addition, 5 ml of water are added to the mixture which is then cooled to 2° to 5° C. The precipitate is separated by filtration and dried to give 0.97 g of the title compound, m.p.: 132°-135° C. The yield is 97% as calculated for 2,6-bis(hydroxymethyl)pyridine. The 2,6-bis(hydroxymethyl)pyridine bis(N-methylcarbamate) content of the thus-obtained product is 98% based on the spectrophotometric determination.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04764613 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-b038f647bb27431aaf565d4a607bf1a4 |
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| 출처 메모 | uspto-grants-1988_08 |
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