Water → HCID 59625513、化合物

HRID 2192836ノート

反応式

HRID 2192836 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH3:15][CH:16]([CH3:32])[CH2:17][NH:18][CH:19]1[CH2:24][CH2:23][CH2:22][N:21]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:20]1.P(C#N)(=O)(OCC)OCC.O>ClCCCl>[NH2:1][C:2]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:3]=1[C:4]([N:18]([CH2:17][CH:16]([CH3:32])[CH3:15])[CH:19]1[CH2:24][CH2:23][CH2:22][N:21]([C:25]([O:27][C:28]([CH3:29])([CH3:30])[CH3:31])=[O:26])[CH2:20]1)=[O:6]

参加物

6

反応物 4

HCID 962WaterHCID 678694-(Trifluoromethyl)anthranilic acidHCID 76257Diethyl cyanophosphonateHCID 59625412HCID 59625412、化合物

生成物 1

HCID 59625513HCID 59625513、化合物収率 47.7%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
70 °C

実験手順

2-amino-4-(trifluoromethyl)benzoic acid (0.32 g) and tert-butyl 3-[(2-methylpropyl)amino]piperidine-1-carboxylate (0.4 g) were dissolved in 1,2-dichloroethane (20 ml), diethyl phosphorocyanidate (0.31 g) was added and the mixture was stirred at 70° C. overnight. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to silica gel column chromatography, and the fraction eluted with ethyl acetate-hexane (0:10-1:1) was concentrated under reduced pressure to give the object compound (0.33 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. washthe fraction eluted with ethyl acetate-hexane (0:10-1:1)
  6. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4a10b225424c4f489865be97580ed51b
出典データセット
uspto-grants-2012_12
特許番号
US08329691B2

反応ノート

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