4-Methoxybenzenesulfonyl chloride → N-[1-(2',5',5-Trifluoro-1,1'-biphenyl-2-yl)ethyl]-4-methoxybenzenesulfonamide

HRID 2181916ノート

反応式

HRID 2181916 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](Cl)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[F:13][C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[C:21]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=1[CH:28]([NH2:30])[CH3:29].C(N(CC)CC)C>>[F:13][C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[C:21]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=1[CH:28]([NH:30][S:9]([C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)(=[O:11])=[O:10])[CH3:29]

参加物

4

反応物 3

HCID 74014-Methoxybenzenesulfonyl chlorideHCID 8471TriethylamineHCID 224822791-(2',5',5-Trifluoro-1,1'-biphenyl-2-yl)ethylamine

生成物 1

HCID 22482378N-[1-(2',5',5-Trifluoro-1,1'-biphenyl-2-yl)ethyl]-4-methoxybenzenesulfonamide収率 91%

実験手順

The title compound was prepared from 4-methoxybenzenesulfonyl chloride (153 mg, 0.74 mmol), 1-(-2′,5′,5-trifluoro-1,1′-biphenyl-2-yl)ethylamine (177 mg, 0.70 mmol), and triethylamine (147 μL, 1.1 mmol) according to the procedure and in the same manner as described in Example 105, step c. The product was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g), eluting with a gradient of 30%-50% methyl tert-butyl ether in hexane (35 min), to afford the desired compound (259 mg, 91%) as a white solid;

後処理

  1. customThe product was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g)
  2. washeluting with a gradient of 30%-50% methyl tert-butyl ether in hexane (35 min)

出典と根拠

ORDレコード
ord-5e7084eab9ce4a138321258104b49a5d
出典データセット
uspto-grants-2005_05
特許番号
US06894061B2

反応ノート

読み込み中…