Diisopropylethylamine → HCID 58930368、化合物

HRID 852432ノート

反応式

HRID 852432 の反応式
CN([CH:4]=[N:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([S:15]([CH3:18])(=[O:17])=[O:16])[CH:10]=1)=[S:7])C.[F:19][C:20]1[CH:29]=[CH:28][CH:27]=[CH:26][C:21]=1[C:22](=[O:25])[CH2:23]Br.C(N(C(C)C)CC)(C)C>CN(C=O)C>[F:19][C:20]1[CH:29]=[CH:28][CH:27]=[CH:26][C:21]=1[C:22]([C:23]1[S:7][C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([S:15]([CH3:18])(=[O:16])=[O:17])[CH:10]=2)=[N:5][CH:4]=1)=[O:25]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 27374492-Bromo-2'-fluoroacetophenoneHCID 724664321-Dimethylaminomethylene-3-(3-methanesulfonyl-phenyl)-thiourea

生成物 1

HCID 58930368HCID 58930368、化合物収率 79%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 37 mg (0.13 mmol) 1-Dimethylaminomethylene-3-(3-methanesulfonyl-phenyl)-thiourea in 0.33 ml DMF was added 28 mg (0.13 mmol) 2-Fluorophenacyl bromide and the mixture was allowed to stir at room temperature for 16 h. 17 mg (0.13 mmol) diisopropylethylamine was added and the mixture was subjected to preparative HPLC separation on reversed phase eluting with an acetonitrile/water gradient to yield 38.5 mg (79%) of the title compound after evaporation of the product fractions.

後処理

  1. customHPLC separation on reversed phase
  2. washeluting with an acetonitrile/water gradient

出典と根拠

ORDレコード
ord-fdb8a297940f4ff0b53f4ac12f606c42
出典データセット
uspto-grants-2007_08
特許番号
US07253197B2

反応ノート

読み込み中…