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Methanesulfonyl chloride → 3-(4-Bromophenyl)propyl methanesulphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-(4-Bromophenyl)propan-1-ol | HCID 10560614 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(4-Bromophenyl)propyl methanesulphonate | HCID 19688466 | 98.9% |
反応手順
To a stirred solution of 3-(4-Bromophenyl)propan-1-ol (500 g, 2.30 mol) and diisopropylethylamine (312 g, 2.40 mol) in anhydrous dichloromethane (4 L) at 0˜5° C. was added dropwise methanesulphonyl chloride (280 g, 2.40 mol) slowly. After addition, the reaction mixture was stirred for 1 hour at 0˜5° C. The reaction mixture was washed with brine (1 L) twice. The organic phase was concentrated in vacuo to afford the subtitle compound (i) (667 g). HPLC Retention Time=1.353 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198285B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-1f92c5e26ddd484ea11e7af9ea1e0168 |
| 出典メモ | uspto-grants-2012_06 |