Potassium Hydroxide → 8-bromo-10H-chromeno[3,2-b]pyridin-10-one

HRID 1409494노트

반응식

HRID 1409494 반응식
[Br:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][C:7]2[C:8]([C:13]#N)=[N:9][CH:10]=[CH:11][CH:12]=2)=[CH:4][CH:3]=1.[OH-:17].[K+]>>[Br:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[C:8](=[N:9][CH:10]=[CH:11][CH:12]=3)[C:13](=[O:17])[C:4]=2[CH:3]=1

참가 물질

3

반응물 2

HCID 14797Potassium HydroxideHCID 667281343-(4-Bromophenoxy)picolinonitrile

생성물 1

HCID 584662358-bromo-10H-chromeno[3,2-b]pyridin-10-one

반응 조건

온도
190 °C

실험 절차

A mixture of 3-(4-bromophenoxy)-picolinonitrile (57 g, 207 mmol) and 300 g of PPA was stirred at 190° C. for 2 h, followed by 180° C. overnight. After cooling to RT, the reaction mixture was poured into 500 g of ice water. After the PH was adjusted to 7 with KOH, the suspension was filtered. The solid was washed with large excess of water, followed by washing with methanol and acetone. The resulting solid was air dried to give 8-bromo-10H-chromeno[3,2-b]pyridin-10-one as a tan solid with >90% purity. The material was carried on to the next step.

후처리

  1. waitfollowed by 180° C. overnight
  2. temperatureAfter cooling to RT
  3. filtrationthe suspension was filtered
  4. washThe solid was washed with large excess of water
  5. washby washing with methanol and acetone
  6. customdried

출처 및 근거

ORD 기록
ord-9eb9f2daeb56473d871fd4e5137f0fe7
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921363B2

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