関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | tert-butyl N-(2-hydroxypropyl)carbamate | HCID 9920508 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Tert-butoxycarbonylamino)propan-2-yl methanesulfonate | HCID 23134071 | — |
反応手順
8.24 g (47.0 mmol) (2-Hydroxy-propyl)-carbamic acid tert-butyl ester were dissolved in 100 ml dichloromethane. 7.8 ml (1.2 equiv.) triethylamine were added and the mixture was cooled to 0° C. At that temperature 4.37 ml (1.2 equiv.) methanesulfonyl chloride were added dropwise. The resulting solution was allowed to reach room temperature and stirred for further 4 h. The mixture was diluted with 100 ml dichloromethane and washed sequentially with a 5% KHSO4-solution, water and brine. The organic phase was dried over anhydrous MgSO4 and concentrated under reduced pressure to give methanesulfonic acid 2-tert-butoxycarbonylamino-1-methyl-ethyl ester in crude form as yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088925B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-449167024039450ea1bd024540009d2a |
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| 出典メモ | uspto-grants-2012_01 |
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