HCID 22054788, 화합물 → HCID 178509714, 화합물

HRID 1829865노트

반응식

HRID 1829865 반응식
[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]

참가 물질

4

반응물 2

HCID 22054788HCID 22054788, 화합물HCID 552656943-Cyano-benzimidic acid methyl ester

생성물 1

HCID 178509714HCID 178509714, 화합물수율 51.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-3619e680be4a45209a8ceb75c2e8b95f
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064142B2

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