참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 반응물 | Tetramethylhexamethylenediamine | HCID 8097 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-(Methylthio)-1-propanol | HCID 10448 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-(Methylthio)propyl 4-methylbenzenesulfonate | HCID 15310998 | 94% |
반응 단계
A solution of 3-(methylthio)-1-propanol (5.30 g, 50.0 mmol), triethylamine (10.5 mL, 75.0 mmol) and N,N,N′,N′-tetramethyl-1,6-hexanediamine (0.861 g, 5.00 mmol) in toluene (50 mL) was ice-cooled, and a solution of p-toluenesulfonyl chloride (14.3 g, 75.0 mmol) in toluene (50 mL) was added dropwise under nitrogen atmosphere. After completion of the dropwise addition, the mixture was stirred for 3 hr, during which the mixture was allowed to warm to room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=10:90-40:60) to give the title compound (12.2 g, yield 94%) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08492430B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-a1cd36ecda794176a7912bc17df2a116 |
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| 출처 메모 | uspto-grants-2013_07 |
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