Cesium carbonate → HCID 86681327, 화합물

HRID 1778920노트

반응식

HRID 1778920 반응식
[O:1]1[C:3]2([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:2]1.[CH3:10][C:11]1[NH:15][C:14]([C:16]#[N:17])=[CH:13][CH:12]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C)C=O.C(OCC)(=O)C>[OH:1][C:3]1([CH2:2][N:15]2[C:11]([CH3:10])=[CH:12][CH:13]=[C:14]2[C:16]#[N:17])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 5706055-Methyl-1H-pyrrole-2-carbonitrileHCID 6429411-Oxaspiro(2.6)nonane

생성물 1

HCID 86681327HCID 86681327, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

1-Oxaspiro[2,6]nonane (2.5 g), 5-methyl-1H-pyrrole-2-carbonitrile (2.1 g) and Cs2CO3 (6.45 g) in N,N-dimethylformamide (15 mL) was heated at 120° C. in a Biotage Initiator microwave reactor for 30 minutes. The reaction mixture was diluted with ethyl acetate, washed with water and concentrated. The residue was purified by reverse phase chromatography, and was eluted with 30%-70% acetonitrile in 0.1% TFA water solution to provide the title compound.

후처리

  1. washwashed with water
  2. concentrationconcentrated
  3. customThe residue was purified by reverse phase chromatography
  4. washwas eluted with 30%-70% acetonitrile in 0.1% TFA water solution

출처 및 근거

ORD 기록
ord-c56891ea55ca4501999b575e23ef7b9a
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266877B2

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