1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 57974945、化合物

HRID 746763

反応式

HRID 746763 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH2:14])=[CH:4][CH:3]=1.C1CCN2C(=NCCC2)CC1.[CH:26]([S:29](Cl)(=[O:31])=[O:30])([CH3:28])[CH3:27]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[NH:14][S:29]([CH:26]([CH3:28])[CH3:27])(=[O:31])=[O:30])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene2 回HCID 824082-Propanesulfonyl chloride2 回HCID 113686332-(4'-Bromophenyl)aniline

生成物 1

HCID 57974945HCID 57974945、化合物収率 75.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Add 4′-bromo-biphenyl-2-ylamine (1.038 g, 4.183 mmol) to CH2Cl2 and cool to 0° C. Add first DBU (2.6 ml, 17.038 mmol), then isopropylsulfonyl chloride (0.95 ml, 8.206 mmol) drop wise to flask and warm flask to room temperature. After 18 hours monitor reaction. If SM is still present, add DBU (1 ml), then isopropylsulfonyl chloride (0.4 ml) and then stir 2 additional hours. Purify resultant product using flash chromatography (Silica gel-25% EtOAc/Hexane) to provide propane-2-sulfonic acid (4′-bromo-biphenyl-2-yl)-amide (1.116 g, 75%). MS(m/e): 351.9(M−1).

後処理

  1. customreaction
  2. customPurify resultant product

出典と根拠

ORDレコード
ord-4d3690aded9b44a298c16f635dbc3d8a
出典データセット
uspto-grants-2008_07
特許番号
US07393868B2

関連ノート

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