Diisopropylethylamine → HCID 59408735、化合物

HRID 1188104ノート

反応式

HRID 1188104 の反応式
[I-].ClC1C=CC=C[N+]=1C.CCN(C(C)C)C(C)C.[C:19]1([CH3:31])[CH:24]=[CH:23][C:22]([C:25]2[S:29][C:28]([NH2:30])=[N:27][CH:26]=2)=[CH:21][CH:20]=1.[Br:32][C:33]1[S:34][C:35]([C:38](O)=[O:39])=[CH:36][N:37]=1>CN(C=O)C.CCOC(C)=O>[Br:32][C:33]1[S:34][C:35]([C:38]([NH:30][C:28]2[S:29][C:25]([C:22]3[CH:21]=[CH:20][C:19]([CH3:31])=[CH:24][CH:23]=3)=[CH:26][N:27]=2)=[O:39])=[CH:36][N:37]=1

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 1670692-Chloro-1-methylpyridinium iodideHCID 9607605-(4-Methylphenyl)-1,3-thiazol-2-amineHCID 27632102-Bromothiazole-5-carboxylic acid

生成物 1

HCID 59408735HCID 59408735、化合物収率 46%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-Chloro-1-methylpyridinium iodide (0.55 g, 2.2 mmol), DIEA (0.37 g, 2.9 mmol) and 5-p-tolylthiazol-2-amine (0.27 g, 1.44 mmol) were added to a suspension of 2-bromothiazole-5-carboxylic acid (0.30 g, 1.44 mmol) in DMF (5 mL). The resulting solution was stirred at RT till completion of the reaction. The mixture was then diluted with AcOEt, washed with water, dried with Na2SO4 and concentrated. The crude product was purified by column (30% AcOEt/PE), yielding 2-bromo-N-(5-p-tolylthiazol-2-yl)thiazole-5-carboxamide (250 mg, 46%) as a solid.

後処理

  1. washwashed with water
  2. dry with materialdried with Na2SO4
  3. concentrationconcentrated
  4. customThe crude product was purified by column (30% AcOEt/PE)

出典と根拠

ORDレコード
ord-47c96296d7324b9c8dab4ccceab79b82
出典データセット
uspto-grants-2014_03
特許番号
US08673940B2

反応ノート

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