Cesium carbonate → HCID 86681327, 화합물

HRID 1430311노트

반응식

HRID 1430311 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-5629e7dc8da14673ab30c43ef994caae
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08940737B2

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