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Methanesulfonyl chloride → 2,8-Diazaspiro[4.5]decane-2-carboxylic acid, 8-(methylsulfonyl)-, 1,1-dimethylethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | tert-Butyl 2,8-diazaspiro[4.5]decane-2-carboxylate | HCID 34178604 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2,8-Diazaspiro[4.5]decane-2-carboxylic acid, 8-(methylsulfonyl)-, 1,1-dimethylethyl ester | HCID 66662714 | 29.6% |
反応手順
To a solution of 2,8-diaza-spiro[4.5]decane-2-carboxylic acid tert-butyl ester (1.12 g, 4.66 mol) in CH2Cl2 (10 ml), triethylamine (3.88 ml) and methanesulfonyl chloride (1.08 ml, 14 mmol) are added at 0° C. The reaction mixture is stirred for overnight, quenched with ice-water and extracted with dichloromethane. The combined extracts are washed with H2O, brine and dried over sodium sulphate to give crude 8-methane sulfonyl-2,8-diaza-spiro[4.5]decane-2-carboxylic acid tert-butyl ester (1.32 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07531546B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-4e5c5d59d83841be87b7ac9a8bc2c62b |
| 出典メモ | uspto-grants-2009_05 |