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Triethylamine → HCID 53734757、化合物

HRID 2187612
ノート
印刷プレビュー

反応式

HRID 2187612 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH:3]=1.[F:19][C:20]1[CH:25]=[CH:24][C:23]([C:26](=O)[CH2:27][N:28]2[CH:32]=[CH:31][N:30]=[CH:29]2)=[CH:22][CH:21]=1.C(N(CC)CC)C.C([BH3-])#N.[Na+].C(=O)([O-])O.[Na+]>ClCCl.CO.[Cl-].[Ti+4].[Cl-].[Cl-].[Cl-]>[F:19][C:20]1[CH:25]=[CH:24][C:23]([CH:26]([NH:1][C:2]2[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=3)[CH:3]=2)[CH2:27][N:28]2[CH:32]=[CH:31][N:30]=[CH:29]2)=[CH:22][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 51512791-(4-fluorophenyl)-2-(1H-imidazol-1-yl)ethan-1-oneHCID 18476027HCID 18476027、化合物

生成物 1

HCID 53734757HCID 53734757、化合物収率 52%

試薬・触媒・溶媒 3

HCID 160960Diamminetetrachlorotitanate(IV)触媒HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

Titanium chloride (2.86 ml; 26 mmol) was added portionwise to a solution of methyl 4-amino-2-(4-fluorophenyl)benzoate (5 g; 20 mmol), 1-(4-fluorophenyl)-2-(imidazol-1-yl) ethanone (4.08 g; 20 mmol) and triethylamine (8.4 ml; 60 mmol) in dichloromethane (120 ml) at 0° C. under argon atmosphere. After stirring overnight at ambient temperature, sodium cyanoborohydride (1.4 g; 0.22 mmol) in solution in methanol (10 ml) was added at 0° C. The reaction mixture was stirred for 2 hours at ambient temperature, treated with 5% aqueous sodium hydrogen carbonate solution, filtered and extracted with dichloromethane. After evaporation to dryness of the organic phase, the residue was purified by flash chromatography eluting with dichloromethane/ethanol 95/5 to give methyl 4-[1-(4-fluorophenyl)-2-(imidazol-1-yl)ethylamino]-2-(4-fluorophenyl)benzoate. Yield 52%.

後処理

  1. stirringThe reaction mixture was stirred for 2 hours at ambient temperature
  2. filtrationfiltered
  3. extractionextracted with dichloromethane
  4. customAfter evaporation to dryness of the organic phase
  5. customthe residue was purified by flash chromatography
  6. washeluting with dichloromethane/ethanol 95/5

出典と根拠

ORDレコード
ord-df3c8ec8df954fa1aee550a7315bab36
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06410539B1

反応ノート

読み込み中…

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