N-bromobutanimide → HCID 22625625、化合物

HRID 277663ノート

反応式

HRID 277663 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:10]=[C:11]2[N:15]([CH:16]=1)[CH2:14][CH2:13][S:12]2.[Br:17]N1C(=O)CCC1=O>CN(C)C=O.O>[Br:17][C:16]1[N:15]2[C:11]([S:12][CH2:13][CH2:14]2)=[N:10][C:9]=1[C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1]

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 141451006-(2,4-Dichlorophenyl)-2,3-dihydroimidazo[2,1-b]thiazole

生成物 1

HCID 22625625HCID 22625625、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

The 6-(2,4-dichlorophenyl)-2,3-dihydroimidazo[2,1-b]thiazole (0.6 g) prepared above and N-bromosuccinimide (0.45 g) were dissolved in dimethylformamide (5 ml). The mixture was heated to reflux and stirred for 18 h at room temperature. The mixture was diluted with water (60 ml) and allowed to crystallize. The liquid was decanted and the residue was dissolved in methylene chloride and dried with magnesium sulfate. The organic residue was chromatographed on silica gel with hexanes/ethyl acetate (3:1) as eluent to give the desired product as a solid (m.p. 200-202° C.); NMR (CDCl3, 200 MHz) δ: 7.4-7.2 (3H), 4.2 (m, 2H), 3.9 (m, 2H).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. customto crystallize
  4. customThe liquid was decanted
  5. dissolutionthe residue was dissolved in methylene chloride
  6. dry with materialdried with magnesium sulfate
  7. customThe organic residue was chromatographed on silica gel with hexanes/ethyl acetate (3:1) as eluent

出典と根拠

ORDレコード
ord-405a007199384286abb5a2b4f9e210e8
出典データセット
uspto-grants-2002_03
特許番号
US06358885B1

反応ノート

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