Hydrochloric Acid → HCID 178432276, 화합물

HRID 513866

반응식

HRID 513866 반응식
[F:1][C:2]1[C:7]2[N:8]=[C:9]([CH3:11])[NH:10][C:6]=2[CH:5]=[C:4]([NH2:12])[CH:3]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[C:23](=[N:36]N)([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.Cl>CN1CCOCC1>[C:23](=[N:36][NH:12][C:4]1[CH:3]=[C:2]([F:1])[C:7]2[NH:8][C:9]([CH3:11])=[N:10][C:6]=2[CH:5]=1)([C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 79304DiphenylmethylidenehydrazineHCID 2733832Lithium HexamethyldisilazideHCID 680053077-fluoro-2-methyl-3H-benzimidazol-5-yl amine

생성물 1

HCID 178432276HCID 178432276, 화합물

시약·촉매·용매 1

HCID 79724-Methylmorpholine용매

반응 조건

온도
100 °C

실험 절차

In a separate reaction container, 7-fluoro-2-methyl-3H-benzimidazol-5-yl amine (100 mg, 0.44 mmol), lithium bis(trimethylsilyl) amide (190 mg, 1.1 mmol), and benzophenone hydrazone (94.3 mg, 0.48 mmol) were dissolved in N-methyl-morpholine (0.5 ml) under a nitrogen atmosphere. Then, the prepared solution containing the catalyst was added thereto. After deaeration, this was heated and stirred at 100° C. under a nitrogen atmosphere for two hours. The reaction mixture was cooled to room temperature, and then an aqueous solution of 6 M hydrochloric acid (0.5 ml) was added thereto. The organic layer was isolated, and concentrated under reduced pressure. Thus, crude N-benzhydrylidene-N′-(7-fluoro-2-methyl-1H-benzimidazol-5-yl)-hydrazine was obtained. The obtained crude product was used in subsequent reactions without being purified.

후처리

  1. additionThen, the prepared solution containing the catalyst
  2. additionwas added
  3. temperatureAfter deaeration, this was heated
  4. temperatureThe reaction mixture was cooled to room temperature
  5. customThe organic layer was isolated
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-153fc8c3594f4a33b3ecfdba3608cf17
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102692B2

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