ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium Carbonate → 1-(2,4-Dichlorophenyl)-N,N-diethyl-3,3-difluoro-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine

HRID 1399144
ノート
印刷プレビュー

反応式

HRID 1399144 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:14]([CH2:15][C:16]([F:20])([F:19])[CH2:17]O)[C:13]2[C:21]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])=[CH:22][CH:23]=[CH:24][C:12]=2[N:11]=1.CS(Cl)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>N1C=CC=CC=1.O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:10]2=[N:11][C:12]3[C:13](=[C:21]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])[CH:22]=[CH:23][CH:24]=3)[N:14]2[CH2:15][C:16]([F:20])([F:19])[CH2:17]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chloride2 回HCID 687716253-{2-[(2,4-Dichlorophenyl)amino]-7-(diethylamino)-1H-benzimidazol-1-yl}-2,2-difluoropropan-1-ol

生成物 1

HCID 577858041-(2,4-Dichlorophenyl)-N,N-diethyl-3,3-difluoro-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine収率 51.3%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

To a solution of 3-{2-[(2,4-dichlorophenyl)amino]-7-(diethylamino)-1H-benzimidazol-1-yl}-2,2-difluoropropan-1-ol (Reference example 154, 48.9 mg, 0.110 mmol) in pyridine (1.5 mL) was added methanesulfonyl chloride (25.6 μL, 0.330 mmol) at 0° C. The mixture was stirred at 0° C. for 2 hrs. The starting material wasn't consumed completely. To the mixture was added methanesulfonyl chloride (25.6 μL, 0.330 mmol) at 0° C. and the mixture was stirred at room temperature for 14 hrs. The mixture was quenched with aqueous sodium hydrogen carbonate and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The resulting mesylate was dissolved into N,N-dimethylformamide (1.5 mL) and to the solution was added potassium carbonate (30.4 mg, 0.220 mmol) at room temperature. The mixture was stirred at 40° C. for 1 hr. After cooling, the mixture was diluted with water and extracted with ethyl acetate. The combined organic layer was washed with water and brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 0-40% ethyl acetate/n-hexane gradient mixture. The resulting solid was recrystallized from hexane to give the title compound as a solid (24.0 mg, 0.0564 mmol, 51%).

後処理

  1. customThe starting material wasn't consumed completely
  2. stirringthe mixture was stirred at room temperature for 14 hrs
  3. customThe mixture was quenched with aqueous sodium hydrogen carbonate
  4. extractionextracted with ethyl acetate
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. dissolutionThe resulting mesylate was dissolved into N,N-dimethylformamide (1.5 mL) and to the solution
  10. stirringThe mixture was stirred at 40° C. for 1 hr
  11. temperatureAfter cooling
  12. extractionextracted with ethyl acetate
  13. washThe combined organic layer was washed with water and brine
  14. dry with materialdried over anhydrous magnesium sulfate
  15. filtrationfiltered
  16. concentrationconcentrated in vacuo
  17. customThe residue was purified by silica gel column chromatography
  18. washeluting with a 0-40% ethyl acetate/n-hexane gradient mixture
  19. customThe resulting solid was recrystallized from hexane

出典と根拠

ORDレコード
ord-277cbc18cddf4c3292856b3957a8c6fe
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901141B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート