P-Toluenesulfonamide → N-4-Tolylsulphonyl-2-[4-(2-butyl-4-chloro-5-formyl-imidazol-1-yl-methyl)-phenyl]-2-cyclopentyl-acetamide
反応式
[CH2:1]([C:5]1[N:6]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([CH:20]([CH:24]3[CH2:28][CH2:27][CH2:26][CH2:25]3)[C:21]([OH:23])=O)=[CH:16][CH:15]=2)[C:7]([CH:11]=[O:12])=[C:8]([Cl:10])[N:9]=1)[CH2:2][CH2:3][CH3:4].C(N(CC)CC)C.S(Cl)(C)(=O)=O.[C:41]1([CH3:51])[CH:46]=[CH:45][C:44]([S:47]([NH2:50])(=[O:49])=[O:48])=[CH:43][CH:42]=1>C1COCC1.CN(C1C=CN=CC=1)C.O.C(O)(=O)C>[C:41]1([CH3:51])[CH:42]=[CH:43][C:44]([S:47]([NH:50][C:21](=[O:23])[CH:20]([C:17]2[CH:18]=[CH:19][C:14]([CH2:13][N:6]3[C:7]([CH:11]=[O:12])=[C:8]([Cl:10])[N:9]=[C:5]3[CH2:1][CH2:2][CH2:3][CH3:4])=[CH:15][CH:16]=2)[CH:24]2[CH2:28][CH2:27][CH2:26][CH2:25]2)(=[O:48])=[O:49])=[CH:45][CH:46]=1参加物
9
反応物 4
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 25 °C
実験手順
1.2 g (2.6 mmol) of the compound from Example II are dissolved in 30 ml of THF, then 0.72 mol (5.2 mmol) of triethylamine, 0.23 ml (2.9 mmol) of mesyl chloride, 320 mg (2.6 mmol) of DMAP and 535 mg (3.1 mmol) of 4-tolylsulphonamide in 10 ml of THF are added successively at 0° C. The mixture is stirred at 25° C. for 20 h, 0.4 ml of glacial acetic acid and 30 ml of water are added, the mixture is extracted three times with 30 ml of ethyl acetate, the organic is phase is concentrated and the residue is chromatographed on silica gel 60 using dichloromethane/methanol (100:2).
後処理
- extractionthe mixture is extracted three times with 30 ml of ethyl acetate
- concentrationis concentrated
- customthe residue is chromatographed on silica gel 60 using dichloromethane/methanol (100:2)
出典と根拠
- ORDレコード
- ord-f151113adc7b4ece8ace9894caf5cc18
- 出典データセット
- uspto-grants-1998_07
- 特許番号
- US05776964
反応ノート
読み込み中…