Phosphorus oxychloride → 7-Bromo-4-chlorothieno[3,2-d]pyrimidine

HRID 532464

反応式

HRID 532464 の反応式
[Br:1][C:2]1[C:6]2[N:7]=[CH:8][NH:9][C:10](=O)[C:5]=2[S:4][CH:3]=1.O=P(Cl)(Cl)[Cl:14]>>[Br:1][C:2]1[C:6]2[N:7]=[CH:8][N:9]=[C:10]([Cl:14])[C:5]=2[S:4][CH:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychloride2 回HCID 1357437127-Bromothieno(3,2-d)pyrimidin-4-ol

生成物 1

HCID 166552667-Bromo-4-chlorothieno[3,2-d]pyrimidine収率 39%

反応条件

温度
150 °C

実験手順

7-bromothieno[3,2-d]pyrimidin-4(3H)-one (5.9 g) was dissolved in POCl3 (20 mL) and the reaction mixture was stirred at 150° C. for 3 hours. The reaction mixture was cooled to room temperature, and remaining POCl3 was concentrated and placed in ice water. The solid thus obtained was washed with sodium bicarbonate and dried using nitrogen gas. The resulting compound was further dried over anhydrous sodium sulfate, and filtered and distilled under reduced pressure to obtain the title compound (1.0 g, 39%).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationwas concentrated
  3. customThe solid thus obtained
  4. washwas washed with sodium bicarbonate
  5. customdried
  6. dry with materialThe resulting compound was further dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-9247ec7529e84e45a198656acda7a568
出典データセット
uspto-grants-2014_10
特許番号
US08853213B2

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