Dimethylformamide diethylacetal → Ethyl 3-(dimethylamino)-2-(5-bromopyridin-3-yl)acrylate

HRID 37894

反応式

HRID 37894 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[N:6][CH:7]=1.C(O[CH:17](OCC)[N:18]([CH3:20])[CH3:19])C>>[CH3:17][N:18]([CH3:20])[CH:19]=[C:8]([C:4]1[CH:5]=[N:6][CH:7]=[C:2]([Br:1])[CH:3]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

3

反応物 2

HCID 70913Dimethylformamide diethylacetalHCID 54116619Ethyl 2-(5-bromopyridin-3-yl)acetate

生成物 1

HCID 68799628Ethyl 3-(dimethylamino)-2-(5-bromopyridin-3-yl)acrylate

実験手順

5.1 g (20.9 mmol) of the compound from Example 10A are stirred in 7.2 ml (6.2 g, 41.8 mmol) of dimethylformamide diethyl acetal at a bath temperature of 100° C. for 16 h. After cooling, the mixture is concentrated under reduced pressure, the residue is stirred in diisopropyl ether, and the solid is filtered off and finally washed with diisopropyl ether. The crude product is dried under reduced pressure for 16 h.

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture is concentrated under reduced pressure
  3. filtrationthe solid is filtered off
  4. washfinally washed with diisopropyl ether
  5. dry with materialThe crude product is dried under reduced pressure for 16 h.

出典と根拠

ORDレコード
ord-fdad1c24727e4b5282819bcce813ea66
出典データセット
uspto-grants-2013_09
特許番号
US08524699B2

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