Water → HCID 67307990、化合物

HRID 404127ノート

反応式

HRID 404127 の反応式
Br[CH2:2][C:3]1[CH:4]=[C:5]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=2)[CH:6]=[CH:7][C:8]=1[CH2:9]Br.C(=O)([O-])[O-].[K+].[K+].[CH3:26][O:27][C:28](=[O:34])[C@H:29]([CH:31]([CH3:33])[CH3:32])[NH2:30].O>C(#N)C>[CH3:32][CH:31]([CH3:33])[CH:29]([N:30]1[CH2:2][C:3]2[C:8](=[CH:7][CH:6]=[C:5]([C:11]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=3)[CH:4]=2)[CH2:9]1)[C:28]([O:27][CH3:26])=[O:34]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 94285Valine methyl esterHCID 673071543,4-bis(Bromomethyl)-4'-nitrobiphenyl

生成物 1

HCID 67307990HCID 67307990、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The compound of example 671 (3 g, 7.79 mmol) was taken in acetonitrile and to the reaction mixture, potassium carbonate (3.25 g, 23.37 mmol) was added followed by the addition of valine methyl ester (1.56 g, 9.35 mmol). The reaction mixture was refluxed for about 16 h and water was added to quench the reaction. The aqueous mixture was extracted with ethyl acetate to obtain a crude material, which was purified using column chromatography (silicagel, 30% ethyl acetate in petroleum ether).

後処理

  1. additionwas added
  2. temperatureThe reaction mixture was refluxed for about 16 h
  3. customto quench
  4. customthe reaction
  5. extractionThe aqueous mixture was extracted with ethyl acetate

出典と根拠

ORDレコード
ord-836010156a004d728a8f4cde327f0724
出典データセット
uspto-grants-2014_06
特許番号
US08748426B2

反応ノート

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