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

HRID 532464

반응식

HRID 532464 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychloride2회HCID 1357437127-Bromothieno(3,2-d)pyrimidin-4-ol

생성물 1

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

반응 조건

온도
150 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9247ec7529e84e45a198656acda7a568
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853213B2

연결된 노트

불러오는 중…