2-Bromopropane → 2-(Isopropylthio)aniline
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].[OH-].[Na+].Br[CH:12]([CH3:14])[CH3:13]>C(O)C>[CH3:13][CH:12]([S:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[NH2:1])[CH3:14]参加物
5
実験手順
To a solution of 2-aminothiophenol (90%, 100 g, 0.72 mol) and sodium hydroxide (31.7 g, 0.792 mol) in 90% aqueous ethanol (500 ml) was added dropwise 2-bromopropane (89 g, 0.72 mol) at room temperature. When the addition was complete, the reaction mixture was refluxed for 3 hours, cooled to room temperature, and then concentrated in vacuo. The residue was diluted with water (300 ml) and extracted with ether (3×500 ml). The ether extracts were washed with water and brine, dried with MgSO4 and concentrated in vacuo to yield the crude product. Distillation through a Vigreaux column gave 2-(1-methylethylthio)benzenamine: bp 94° (2.2-2.4 mm).
後処理
- additionWhen the addition
- temperaturethe reaction mixture was refluxed for 3 hours
- concentrationconcentrated in vacuo
- additionThe residue was diluted with water (300 ml)
- extractionextracted with ether (3×500 ml)
- washThe ether extracts were washed with water and brine
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
- customto yield the crude product
- distillationDistillation through a Vigreaux column
出典と根拠
- ORDレコード
- ord-305229975b5d41778d487869b6f2061c
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04818277
反応ノート
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