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Sulfuric Acid → 1-Bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| 反応物 | 1,1-Dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene | HCID 19931783 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene | HCID 19931768 | 12,381.4% |
反応手順
A suspension of Triton B (Reg Trade Mark, N-benzyltrimethylammonium hydroxide, 40% in methanol, 1.8 g) in toluene was added to a solution of 1,1-dibromo-2-[2-chloro-4-(methylsulphenyl)phenyl]ethene (0.96 g) in toluene. The mixture was stirred for 15 minutes. Sulphuric acid (2 m) was added and the resulting layers were separated. The organic layer was washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromotography eluted with a mixture of hexane and dichloromethane to give 1-bromo-2-[2-chloro-4-(methylsulphenyl)phenyl]acetylene 90.78 g) as a yellow oil, NMR (CDCl3) 2.5 (s,3H), 7.05(d,1H), 7.2(s,1H), 7.35(d,1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424276 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-f5d5be1f25384852af0050db91e2a0fa |
| 出典メモ | uspto-grants-1995_06 |