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 [4-(2-hydroxyethyl)phenoxy]acetate | HCID 23119602 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl (4-{2-[(methylsulfonyl)oxy]ethyl}phenoxy)acetate | HCID 86600965 | 95.5% |
反応手順
Tert-butyl [4-(2-hydroxyethyl)phenoxy]acetate (6.000 g, 23.781 mmol) and triethylamine (9.9 ml, 71.341 mmol) were dissolved in DCM. The mixture was cooled to −10° C. and methanesulfonyl chloride (2.8 ml, 35.671 mmol) was added dropwise to the mixture. The reaction mixture was allowed to reach room temperature and was stirred for 16 hours. The mixture was diluted with DCM. The organic layer was washed with water, brine and 0.3M KHSO4, dried with MgSO4, and evaporated under reduced pressure. Obtained 7.5 g of light-yellow crystals (yield 95.5%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07351858B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-645b4593cacc44a79a13e29e22ae538e |
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| 出典メモ | uspto-grants-2008_04 |
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