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Einecs 211-027-4 → CID 117760255

HRID 709610
ノート
印刷プレビュー

反応式

HRID 709610 の反応式
[CH:1]1([CH:4]([C:11]2[CH:16]=[C:15]([O:17]C)[N:14]=[CH:13][N:12]=2)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3][CH2:2]1.[Cl-].[NH+]1C=CC=CC=1.C(=O)([O-])O.[Na+]>CN(C=O)C.C(#N)C>[CH:1]1([CH:4]([C:11]2[CH:16]=[C:15]([OH:17])[N:14]=[CH:13][N:12]=2)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 69401Einecs 211-027-4HCID 516892Sodium BicarbonateHCID 117760142Ethyl 3-cyclopropyl-3-(6-methoxypyrimidin-4-yl)propanoate

生成物 1

HCID 178471101CID 117760255

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
130 °C

実験手順

Under a nitrogen atmosphere, to a solution of ethyl 3-cyclopropyl-3-(6-methoxypyrimidin-4-yl)propanoate (entire amount) in DMF (15 mL) was added pyridinium chloride (25.9 g), and the mixture was stirred at 130° C. for 20 min. The reaction mixture was cooled to 0° C. and diluted with acetonitrile (20 mL). Sodium hydrogen carbonate (17.0 g) was added to the reaction mixture, the insoluble material was filtered off, and the solvent in the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane), and the obtained solid was washed with diisopropyl ether to give the title compound (3.66 g) as a white solid.

後処理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. filtrationthe insoluble material was filtered off
  3. customthe solvent in the filtrate was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  5. washthe obtained solid was washed with diisopropyl ether

出典と根拠

ORDレコード
ord-e6dc28229f74484fa35d70feccfd64c6
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181186B2

反応ノート

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