Hydrochloric Acid → HCID 178432276、化合物

HRID 513866

反応式

HRID 513866 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 178432276HCID 178432276、化合物

試薬・触媒・溶媒 1

HCID 79724-Methylmorpholine溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-153fc8c3594f4a33b3ecfdba3608cf17
出典データセット
uspto-grants-2015_08
特許番号
US09102692B2

関連ノート

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