Phosphorus oxybromide → 4-Bromo-1,5-naphthyridine

HRID 1253510ノート

反応式

HRID 1253510 の反応式
[N:1]1[C:10]2[C:5](=[N:6][CH:7]=[CH:8][CH:9]=2)[C:4](O)=[CH:3][CH:2]=1.P(Br)(Br)([Br:14])=O>>[Br:14][C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][N:6]=2)[N:1]=[CH:2][CH:3]=1

参加物

3

反応条件

温度
150 °C

実験手順

A flask was charged with 1,5-naphthyridin-4-ol (1 g, 6.7 mmol) and phosphorousoxybromide (5 g, 17 mmol). The mixture was heated to 150° C., stirred for 1 hour, and then cooled to room temperature. The mixture was poured into ice-water and extracted with toluene. The combined organic extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to give crude product, which was re-crystallized from petroleum ether to give 4-bromo-1,5-naphthyridine.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with toluene
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give crude product, which
  8. customwas re-crystallized from petroleum ether

出典と根拠

ORDレコード
ord-221d1e0d305a498c93b370d8baa12e97
出典データセット
uspto-grants-2013_06
特許番号
US08455477B2

反応ノート

読み込み中…