참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 1-(4-Nitrophenyl)ethan-1-ol | HCID 592376 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(4-Nitrophenyl)ethyl methanesulfonate | HCID 11218799 | 91% |
반응 단계
(a-1) To a stirred solution of 50.2 parts of α-methyl-4-nitrobenzenemethanol and 48.6 parts of N,N-diethylethanamine in 390 parts of dry dichloromethane was added dropwise a solution of 37.8 parts of methanesulfonyl chloride in 65 parts of dry dichloromethane at -5~0° C. The whole was stirred for 1 hour at 0° C. 75 Parts of cold water were added and the dichloromethane layer was decanted, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated. The solid residue was shaked with 2,2'-oxybispropane. The product was filtered off and dried, yielding 67.1 parts (91%) of [1-(4-nitrophenyl)ethyl] methanesulfonate; mp. 70° C. (int. 112).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04859684 |
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| 출처 데이터셋 | uspto-grants-1989_08 |
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| ORD ID | ord-2075c749647943ad8da232aedf83b613 |
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| 출처 메모 | uspto-grants-1989_08 |
|---|