5-(5-Bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione → (5-Bromopyridin-2-yl)acetic acid

HRID 533505ノート

反応式

HRID 533505 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[C:8]2C(=O)OC(C)(C)[O:10][C:9]2=[O:17])[NH:6][CH:7]=1>Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([OH:17])=[O:10])=[N:6][CH:7]=1

参加物

3

実験手順

A solution of 5-(5-bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3) (40.0 g, 133.3 mmol) in HCl (30%, 400 mL) was heated gently to reflux, and was refluxed for 2 h. The solvent was removed in vacuo and the residue (29.75 g) was used in the next step without further purification. 1H-NMR (CDCl3, 300 MHz): δ 3.79 (s, 2H, CH2), 7.41 (d, 1H, ArH), 8.08 (dd, 1H, ArH), 8.66 (d, 1H, ArH).

後処理

  1. temperatureto reflux
  2. temperaturewas refluxed for 2 h
  3. customThe solvent was removed in vacuo
  4. customthe residue (29.75 g) was used in the next step without further purification

出典と根拠

ORDレコード
ord-ed9b94004346481598f2462e27f3012f
出典データセット
uspto-grants-2014_10
特許番号
US08853258B2

反応ノート

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