Water → HCID 59850131、化合物

HRID 2064161ノート

反応式

HRID 2064161 の反応式
F[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([C:9]([F:12])([F:11])[F:10])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].C(N(C(C)C)CC)(C)C.[NH2:25][CH:26]1[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:28][CH2:27]1.O>CN(C)C=O>[CH3:8][C:6]1[C:5]([C:9]([F:12])([F:11])[F:10])=[CH:4][C:3]([N+:13]([O-:15])=[O:14])=[C:2]([NH:25][CH:26]2[CH2:27][CH2:28][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:30][CH2:31]2)[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 12682914-Amino-1-Boc-piperidineHCID 598501821-Fluoro-5-methyl-2-nitro-4-(trifluoromethyl)benzene

生成物 1

HCID 59850131HCID 59850131、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

1-Fluoro-5-methyl-2-nitro-4-(trifluoromethyl)benzene (D56) (4.9 mmol, 1.1 g) was dissolved in dry dimethylformamide (3 ml) and diisopropylethylamine (1 eq., 4.9 mmol, 0.460 ml), 1,1-dimethylethyl 4-amino-1-piperidinecarboxylate (1 eq., 4.9 mmol, 981 mg) were added at room temperature and the mixture was stirred at 80° C. for 3 hours. The crude mixture was then cooled to room temperature and water was added; the aqueous solution was extracted with ethyl acetate; organics were alternatively washed with brine and water. The organics were combined dried over Na2SO4, filtered and the solvent was evaporated to afford the crude compound that was purified by chromatography (ethyl acetate-n-hexane) to yield the title compound, 1.29 g, 65%, M+−H=402.

後処理

  1. extractionthe aqueous solution was extracted with ethyl acetate
  2. washorganics were alternatively washed with brine and water
  3. dry with materialThe organics were combined dried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customto afford the crude compound that
  7. customwas purified by chromatography (ethyl acetate-n-hexane)

出典と根拠

ORDレコード
ord-fa7c88752b9e4c4099cd185f2231bfff
出典データセット
uspto-grants-2012_10
特許番号
US08288412B2

反応ノート

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