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Water → HCID 58355471、化合物

HRID 1509430
ノート
印刷プレビュー

反応式

HRID 1509430 の反応式
Cl[C:2](Cl)(Cl)[C:3]1[NH:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[N:4]=1.[CH3:14][CH:15]([CH3:35])[CH2:16][NH:17][C@@H:18]1[CH2:23][N:22]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:21][C@H:20]([C:31]([O:33][CH3:34])=[O:32])[CH2:19]1.C(=O)([O-])[OH:37].[Na+].O>C1COCC1>[NH:4]1[C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=[C:3]1[C:2]([N:17]([CH2:16][CH:15]([CH3:35])[CH3:14])[C@@H:18]1[CH2:23][N:22]([C:24]([O:26][C:27]([CH3:29])([CH3:30])[CH3:28])=[O:25])[CH2:21][C@H:20]([C:31]([O:33][CH3:34])=[O:32])[CH2:19]1)=[O:37]
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 4

HCID 962WaterHCID 77133Benzimidazole, 2-trichloromethyl-HCID 516892Sodium BicarbonateHCID 593566071-tert-butyl 3-methyl (3R,5S)-5-[(2-methylpropyl)amino]piperidine-1,3-dicarboxylate

生成物 1

HCID 58355471HCID 58355471、化合物収率 83.9%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
50 °C

実験手順

2-(Trichloromethyl)-1H-benzimidazole (19 g) and 1-tert-butyl 3-methyl (3R,5S)-5-[(2-methylpropyl)amino]piperidine-1,3-dicarboxylate (25 g) were dissolved in THF (1200 ml), sodium hydrogen carbonate (67 g) and water (600 ml) were added, and the mixture was stirred at room temperature for 1 hr and at 50° C. for 1 hr. After evaporation of the solvent, the residue was extracted 3 times with ethyl acetate (700 ml). The extract was washed successively with 10%-aqueous citric acid solution (500 ml) and brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate (1000 ml), subjected to basic silica gel column chromatography, and a fraction eluted with ethyl acetate was concentrated under reduced pressure to give the object product (30.6 g).

後処理

  1. customAfter evaporation of the solvent
  2. extractionthe residue was extracted 3 times with ethyl acetate (700 ml)
  3. washThe extract was washed successively with 10%-aqueous citric acid solution (500 ml) and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. dissolutionThe residue was dissolved in ethyl acetate (1000 ml)
  7. washa fraction eluted with ethyl acetate
  8. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f83d99345eab465a809047f77863dc02
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221836B2

反応ノート

読み込み中…

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