Triethylamine → N'-[5-(2-chloro-benzoyl)-thiazol-2-yl]-N,N-dimethyl-formamidine

HRID 529983ノート

反応式

HRID 529983 の反応式
[NH2:1][C:2]([NH2:4])=[S:3].CO[CH:7]([N:10]([CH3:12])[CH3:11])OC.[CH2:13](N(CC)CC)C.Br[CH2:21][C:22]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[Cl:30])=[O:23]>CO>[Cl:30][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=1[C:22]([C:21]1[S:3][C:2]([N:4]=[CH:12][N:10]([CH3:7])[CH3:11])=[N:1][CH:13]=1)=[O:23]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 78373Dimethylformamide dimethyl acetalHCID 2723790ThioureaHCID 27357852-Bromo-2'-chloroacetophenone

生成物 1

HCID 66628633N'-[5-(2-chloro-benzoyl)-thiazol-2-yl]-N,N-dimethyl-formamidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture of thiourea (4.95 g, 65.0 mmol) and dimethoxymethyl-dimethyl-amine (23.2 g, 195 mmol) in methanol (80 mL) was heated to reflux for 30 minutes. After allowing the mixture to cool, triethylamine (19.8 g, 195 mmol) and a solution of 2-bromo-1-(chloro-phenyl)-ethanone (crude from last step) in methanol (50 mL) were added. The mixture was heated to reflux for 4 hours. The solvent was removed and the residue was used directly in the next procedure.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 30 minutes
  3. temperatureto cool
  4. temperatureThe mixture was heated
  5. temperatureto reflux for 4 hours
  6. customThe solvent was removed

出典と根拠

ORDレコード
ord-cf80008316be462a946c8c8f4ead7804
出典データセット
uspto-grants-2016_05
特許番号
US09351962B2

反応ノート

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