Potassium Hydroxide → HCID 10913596、化合物

HRID 1264563ノート

反応式

HRID 1264563 の反応式
[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

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 18612501HCID 18612501、化合物

生成物 1

HCID 10913596HCID 10913596、化合物収率 90%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-de9550cbafba4e248c8fa6f863a27025
出典データセット
uspto-grants-2003_04
特許番号
US06544979B1

反応ノート

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