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Bromine → 2-bromo-3-hexyl-5,5-dimethyl-6,7,8,9-tetrahydro-5H-benzocycloheptene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2-hexyl-9,9-dimethyl-6,7,8,9-tetrahydro-5H-benzocycloheptene | HCID 21846716 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-bromo-3-hexyl-5,5-dimethyl-6,7,8,9-tetrahydro-5H-benzocycloheptene | HCID 21846719 | — |
反応手順
This 3.08 g of 2-hexyl-9,9-dimethyl-6,7,8,9-tetrahydro-5H-benzocycloheptene were dissolved in 35 ml of CH2Cl2, treated at 0° with a spatula tip of Fe powder and then reacted with a solution of 0.67 ml of Br2 (1.1 eq.) in 5 ml of CH2Cl2. After 30 min., the mixture was poured on to ice, extracted with diethyl ether, washed with bisulphite solution and NaCl soln., dried over Na2SO4 and evaporated to dryness. Flash chromatography on SiO2 (hexane) gave 3.21 g of 2-bromo-3-hexyl-5,5-dimethyl-6,7,8,9-tetrahydro-5H-benzocycloheptene as a colorless oil (GC purity: 82%, moreover 2% ed., 2.6% regioisomer, 8.3% dibromo compound and further prod.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726191 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-f15578709608425ca7e804635f32e399 |
| 出典メモ | uspto-grants-1998_03 |