反応式
[S:1]([C:21]1[CH:26]=C(C2C(Cl)=CC(C(F)(F)F)=CC=2Cl)C=C[C:22]=1C)[C:2]1[CH:7]=[C:6]([C:8]2[C:13]([Cl:14])=[CH:12][C:11]([C:15]([F:18])([F:17])[F:16])=[CH:10][C:9]=2[Cl:19])[CH:5]=[CH:4][C:3]=1[CH3:20].C(S([O-])=O)O.[Na+].C(I)(C)C.O>CN(C)C=O>[CH:21]([S:1][C:2]1[CH:7]=[C:6]([C:8]2[C:9]([Cl:19])=[CH:10][C:11]([C:15]([F:18])([F:16])[F:17])=[CH:12][C:13]=2[Cl:14])[CH:5]=[CH:4][C:3]=1[CH3:20])([CH3:26])[CH3:22]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
3.3 g (4.9 mmol) of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene], 3.0 g (19.5 mmol) of Rongalite and 3.0 g (17.6 mmol) of isopropyl iodide were stirred in 30 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.4 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylphenyl] isopropyl sulfide (yield 38.0%) as a yellow dough (nD20 1.5462).
後処理
- customThe resulting reaction mixture
- extractionextracted with 50 ml of ethyl acetate twice
- washThe ethyl acetate layer was washed with 50 ml of water twice
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe ethyl acetate was distilled off under reduced pressure
- customPurification of the residue by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-0fbc315e828d4f1596636d7f04b90a6e
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07767626B2
関連ノート
読み込み中…