Cesium carbonate → HCID 86681327、化合物

HRID 1778920ノート

反応式

HRID 1778920 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 86681327HCID 86681327、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c56891ea55ca4501999b575e23ef7b9a
出典データセット
uspto-grants-2016_02
特許番号
US09266877B2

反応ノート

読み込み中…