Potassium Hydroxide → HCID 10913596, 화합물

HRID 1016371노트

반응식

HRID 1016371 반응식
[Cl:1][C:2]1[N:11]2[C:5]([C:6](=[C:16]3[CH2:21][CH2:20][N:19](C(OCC)=O)[CH2:18][CH2:17]3)[C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH2:9][CH2:10]2)=[N:4][CH:3]=1.[OH-].[K+]>C(O)(C)C>[Cl:1][C:2]1[N:11]2[C:5]([C:6](=[C:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH2:9][CH2:10]2)=[N:4][CH:3]=1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 18612501HCID 18612501, 화합물

생성물 1

HCID 10913596HCID 10913596, 화합물수율 90%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of intermediate 12 (30.4 g) and potassium hydroxide (46 g) in isopropanol (370 ml) was stirred and refluxed for 6 hours. The solvent was evaporated. The residue was taken up in water and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from ACN. The precipitate was filtered off and dried, yielding 1.65 g (90%) of 3-chloro-6,11-dihydro-11-(4-piperidinylidene)-5H-imidazo[2,1-b][3]benzazepine (intermediate 13).

후처리

  1. temperaturerefluxed for 6 hours
  2. customThe solvent was evaporated
  3. extractionextracted with DCM
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was crystallized from ACN
  9. filtrationThe precipitate was filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-c45726d8b9aa48dda20ccda4381ba9e1
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06476018B1

반응 노트

불러오는 중…