Ammonium Chloride → HCID 71258209, 화합물

HRID 1506216노트

반응식

HRID 1506216 반응식
[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

참가 물질

4

반응물 2

HCID 25517Ammonium ChlorideHCID 86726636HCID 86726636, 화합물

생성물 1

HCID 71258209HCID 71258209, 화합물수율 74%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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%).

후처리

  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))

출처 및 근거

ORD 기록
ord-43731ace86af43a0b3913bdba1a2a689
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216999B2

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