Ammonium Chloride → HCID 71258209、化合物

HRID 1506216ノート

反応式

HRID 1506216 の反応式
[CH:1]1([NH:7][C:8]2[C:13]([C:14]([NH:16][CH:17]=O)=[O:15])=[CH:12][N:11]=[C:10]3[N:19]([CH2:22][O:23][CH2:24][CH2:25][Si:26]([CH3:29])([CH3:28])[CH3:27])[CH:20]=[CH:21][C:9]=23)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl-].[NH4+]>CN1CCCC1=O>[CH:1]1([N:7]2[C:8]3[C:9]4[CH:21]=[CH:20][N:19]([CH2:22][O:23][CH2:24][CH2:25][Si:26]([CH3:28])([CH3:27])[CH3:29])[C:10]=4[N:11]=[CH:12][C:13]=3[C:14](=[O:15])[N:16]=[CH:17]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 25517Ammonium ChlorideHCID 86726636HCID 86726636、化合物

生成物 1

HCID 71258209HCID 71258209、化合物収率 74%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

4-(Cyclohexylamino)-N-formyl-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine-5-carboxamide (12.4 mg, 0.0311 mmol) in N-methyl-2-pyrrolidinone (0.5 mL) was stirred at 200° C. for 30 minutes under microwave irradiation. The reaction mixture was allowed to cool to room temperature and, after addition of saturated aqueous ammonium chloride, extracted with ethyl acetate, and the organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1 (v/v)) to give the title compound as a pale yellow amorphous (9.2 mg, yield 74%).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1 (v/v))

出典と根拠

ORDレコード
ord-43731ace86af43a0b3913bdba1a2a689
出典データセット
uspto-grants-2015_12
特許番号
US09216999B2

反応ノート

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