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Dimethylformamide → N-[(5-chloro-1-methyl-1H-benzimidazol-2-yl)methyl]-2-(5-chloro-2-oxo-1,3-benzothiazol-3 (2H)-yl)-N-methylacetamide hydrochloride

HRID 1428410
ノート
印刷プレビュー

反応式

HRID 1428410 の反応式
[H-].[Na+].[CH3:3]N(C=O)C.[Cl:8][C:9]1[CH:34]=[CH:33][C:12]2[NH:13][C:14]([CH2:16][N:17]([CH3:32])[C:18](=[O:31])[CH2:19][N:20]3[C:24]4[CH:25]=[C:26]([Cl:29])[CH:27]=[CH:28][C:23]=4[S:22][C:21]3=[O:30])=[N:15][C:11]=2[CH:10]=1.CI>O>[ClH:8].[Cl:8][C:9]1[CH:34]=[CH:33][C:12]2[N:13]([CH3:3])[C:14]([CH2:16][N:17]([CH3:32])[C:18](=[O:31])[CH2:19][N:20]3[C:24]4[CH:25]=[C:26]([Cl:29])[CH:27]=[CH:28][C:23]=4[S:22][C:21]3=[O:30])=[N:15][C:11]=2[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 178483012HCID 178483012、化合物

生成物 1

HCID 117652655N-[(5-chloro-1-methyl-1H-benzimidazol-2-yl)methyl]-2-(5-chloro-2-oxo-1,3-benzothiazol-3 (2H)-yl)-N-methylacetamide hydrochloride

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

Under a nitrogen gas flow, to a mixture of NaH (55% in oil, 35 mg) and DMF (4 mL) was added a mixture of N-[(5-chloro-1H-benzimidazol-2-yl)methyl]-2-(5-chloro-2-oxo-1,3-benzothiazol-3(2H)-yl)-N-methylacetamide (335 mg) and DMF (10 mL) under ice-cooling, followed by stirring at room temperature for 30 minutes. The reaction mixture was ice-cooled and methyl iodide (55 μL) was added thereto, followed by stirring at room temperature overnight. The reaction mixture was added to water, followed by extraction with EtOAc. The organic layer was washed with brine and dried over Na2SO4, and then concentrated under reduced pressure. To the residue was added chloroform. The resulting solid was collected and then washed with chloroform. To a mixture of the obtained solid and MeOH (3 mL) was added 4 M hydrogen chloride/EtOAc (300 μL), followed by stirring at room temperature. The reaction mixture was concentrated under reduced pressure, and to the residue was added EtOAc. The resulting solid was collected and then washed with EtOAc to obtain N-[(5-chloro-1-methyl-1H-benzimidazol-2-yl)methyl]-2-(5-chloro-2-oxo-1,3-benzothiazol-3(2H)-yl)-N-methylacetamide hydrochloride (60 mg).

後処理

  1. additionwas added
  2. temperaturecooling
  3. temperaturecooled
  4. stirringby stirring at room temperature overnight
  5. extractionfollowed by extraction with EtOAc
  6. washThe organic layer was washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated under reduced pressure
  9. additionTo the residue was added chloroform
  10. customThe resulting solid was collected
  11. washwashed with chloroform
  12. additionTo a mixture of the obtained solid and MeOH (3 mL)
  13. additionwas added 4 M hydrogen chloride/EtOAc (300 μL)
  14. stirringby stirring at room temperature
  15. concentrationThe reaction mixture was concentrated under reduced pressure
  16. additionto the residue was added EtOAc
  17. customThe resulting solid was collected
  18. washwashed with EtOAc

出典と根拠

ORDレコード
ord-eec89834c44e4379accad58d28012a2d
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937087B2

反応ノート

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