反応式
Cl.[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[C:10](=[O:17])[CH2:11][N:12]1[CH:16]=[N:15][CH:14]=[N:13]1.[I-].[CH3:19][S+:20]([CH3:23])(C)=[O:21].[OH-:24].[Na+]>C1(C)C=CC=CC=1.CCCCCCCCCCCCCC[N+](C)(C)C>[CH3:23][S:20]([OH:17])(=[O:21])=[O:24].[F:2][C:3]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:4]=1[C:10]1([O:17][CH2:19]1)[CH2:11][N:12]1[CH:16]=[N:15][CH:14]=[N:13]1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 0 °C
実験手順
2',4'-Difluoro-2-(1H-1,2,4-triazol-1-yl)acetophenone hydrochloride (59.6 g, 0.23M), trimethylsulphoxonium iodide (50.6 g, 0.23M) and cetrimide (2.1 g) were stirred in a mixture of toluene (370 ml) and 20% w/w aqueous sodium hydroxide at 60° for 3 hours. The toluene layer was separated and concentrated to 110 ml then diluted with ethyl acetate (150 ml). A solution of methanesulphonic acid (16.6 g, 0.172M) in ethyl acetate (20 ml) was added. More ethyl acetate (100 ml) was added and the mixture was stirred at 0° C. for one hour then filtration of the precipitate gave the title compound (43 g, 56%).
後処理
- customThe toluene layer was separated
- concentrationconcentrated to 110 ml
- additionthen diluted with ethyl acetate (150 ml)
- additionA solution of methanesulphonic acid (16.6 g, 0.172M) in ethyl acetate (20 ml) was added
- additionMore ethyl acetate (100 ml) was added
- filtrationfiltration of the precipitate
出典と根拠
- ORDレコード
- ord-0f30691268ca44be918bb9d9fd101fac
- 出典データセット
- uspto-grants-1987_04
- 特許番号
- US04661507
関連ノート
読み込み中…