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Chlorosulfonic acid → 5-Bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 5-Bromo-2-methyl-2,3-dihydro-1-benzofuran | HCID 13301601 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-Bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochloride | HCID 86741176 | 65% |
反応手順
470 g (4.03 moles) of chlorosulfonic acid are added dropwise over 20 minutes at -7° C. to a solution of 106 g (0.5 mole) of 5-bromo-2,3-dihydro-2-methylbenzo[b]furan in 300 ml of chloroform, and the mixture is then stirred for a further 15 minutes at 20°-25° C. The reaction mixture is taken up in ice/water, the organic phase is separated, and aqueous phase is extracted with two 500 ml portions of chloroform. The combined organic phases are washed with two 250 ml portions of water, dried over sodium sulfate, and concentrated, affording 101 g (65% of theory) of 5-bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04634465 |
| 出典データセット | uspto-grants-1987_01 |
| ORD ID | ord-4cb0146883cb465d958a1de54e18d073 |
| 出典メモ | uspto-grants-1987_01 |