HCID 23362032、化合物 → HCID 68762744、化合物

HRID 1398935ノート

反応式

HRID 1398935 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](N)[C:3]=1[NH:9][CH2:10][CH2:11][OH:12].Cl.[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=1[CH:22]([OH:27])[C:23](=[NH:26])OC>C(O)C.C(=O)([O-])O.[Na+]>[NH2:1][C:2]1[C:3]2[N:9]([CH2:10][CH2:11][OH:12])[C:23]([CH:22]([C:16]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:15]=3[Cl:14])[OH:27])=[N:26][C:4]=2[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 23362032HCID 23362032、化合物HCID 68736952HCID 68736952、化合物

生成物 1

HCID 68762744HCID 68762744、化合物収率 99.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a stirred solution of 2-[(2,6-diaminophenyl)amino]ethanol (3.63 g, 21.7 mmol) in ethanol (43 mL) was added methyl 2-(2,4-dichlorophenyl)-2-hydroxyethanimidoate hydrochloride (7.04 g, 26.0 mmol) at room temperature. After 12 h, the reaction mixture was diluted with aqueous sodium hydrogen carbonate. The resultant mixture was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with ethyl acetate to give the title compound as an orange amorphous solid (7.58 g, 21.5 mmol, 99%).

後処理

  1. extractionThe resultant mixture was extracted with ethyl acetate
  2. washThe combined organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography on silica gel eluting with ethyl acetate

出典と根拠

ORDレコード
ord-3f6a9aa63cfe46e6b8c1cff0419962e0
出典データセット
uspto-grants-2014_12
特許番号
US08901141B2

反応ノート

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