HCID 22054788、化合物 → HCID 178509714、化合物

HRID 1829865ノート

反応式

HRID 1829865 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)([NH2:11])[CH2:9][NH2:10])=[CH:4][CH:3]=1.CO[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([C:29]#N)[CH:24]=1)=[NH:22]>CO>[C:21]([C:23]1[CH:24]=[C:25]([C:29]2[NH:10][CH2:9][C:8]([C:12]3[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=3)([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)[N:11]=2)[CH:26]=[CH:27][CH:28]=1)#[N:22]

参加物

4

反応物 2

HCID 22054788HCID 22054788、化合物HCID 552656943-Cyano-benzimidic acid methyl ester

生成物 1

HCID 178509714HCID 178509714、化合物収率 51.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1,1-bis(4-fluorophenyl)-1,2-ethanediamine (500 mg) in methanol (10 mL) was added 3-cyanobenzeneimidic acid methyl ester (792 mg), and the mixture was stirred at room temperature for 18 hrs. After concentrating the reaction mixture, the residue was dissolved in ethyl acetate (30 mL), washed with saturated sodium hydrogen carbonate aqueous solution and saturated sodium chloride aqueous solution in this order, and dried over anhydrous sodium sulfate. Sodium sulfate was removed by filtration, and the organic solvent was evaporated in vacuo. The obtained residue was purified by silica gel column chromatography (C-300; hexane:ethyl acetate=3:1→2:1) to give the objective compound (370 mg).

後処理

  1. concentrationAfter concentrating the reaction mixture
  2. dissolutionthe residue was dissolved in ethyl acetate (30 mL)
  3. washwashed with saturated sodium hydrogen carbonate aqueous solution and saturated sodium chloride aqueous solution in this order
  4. dry with materialdried over anhydrous sodium sulfate
  5. customSodium sulfate was removed by filtration
  6. customthe organic solvent was evaporated in vacuo
  7. customThe obtained residue was purified by silica gel column chromatography (C-300; hexane:ethyl acetate=3:1→2:1)

出典と根拠

ORDレコード
ord-3619e680be4a45209a8ceb75c2e8b95f
出典データセット
uspto-grants-2006_06
特許番号
US07064142B2

反応ノート

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