참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Guaifenesin | HCID 3516 | — |
| 반응물 | N-Methylsulfamoyl chloride | HCID 11789235 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 53888739 | HCID 53888739 | 37% |
반응 단계
A solution of 26.5 g (0.13 mole) of glycerol guaiacolate in 100 ml of methylene chloride and 10.8 ml (0.13 mole) of pyridine was added in a thin stream to a stirred solution of 17.1 g (0.13 mole) of N-methylsulfamoyl chloride (Preparation 24) in 70 ml of methylene chloride, and the reaction mixture was stirred at ambient temperature for 2 hr. The reaction mixture was treated with 150 ml of water, the layers were separated, and the organic layer was washed successively with a 200 ml portion of 2N hydrochloric acid solution, four 200 ml portions of water, dried (magnesium sulfate), and the solvent was evaporated under reduced pressure to yield a viscous oil. The oil was purified by preparative high pressure liquid chromatography. Fractions containing the desired product were combined and the solvents evaporated under reduced pressure to give 13.9 g (37%) of the title compound as a yellow gum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05273993 |
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| 출처 데이터셋 | uspto-grants-1993_12 |
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| ORD ID | ord-97ec3988ea2d4813aff2b3593cae75cd |
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| 출처 메모 | uspto-grants-1993_12 |
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