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Ammonium Hydroxide → Seganserin

HRID 1980150
ノート
印刷プレビュー

反応式

HRID 1980150 の反応式
Cl.Cl.[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([C:31]2[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=2)=[C:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][C:19]3[C:24](=[O:25])[N:23]4[CH:26]=[CH:27][CH:28]=[CH:29][C:22]4=[N:21][C:20]=3[CH3:30])[CH2:13][CH2:12]2)=[CH:6][CH:5]=1.[OH-].[NH4+]>O>[F:37][C:34]1[CH:35]=[CH:36][C:31]([C:10]([C:7]2[CH:6]=[CH:5][C:4]([F:3])=[CH:9][CH:8]=2)=[C:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][C:19]3[C:24](=[O:25])[N:23]4[CH:26]=[CH:27][CH:28]=[CH:29][C:22]4=[N:21][C:20]=3[CH3:30])[CH2:15][CH2:16]2)=[CH:32][CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 159037R-56413

生成物 1

HCID 71767Seganserin

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5 Parts of 3-[2-[4-[bis(4-fluorophenyl)methylene]-1-piperidinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one dihydrochloride were dissolved in water and the base was liberated with ammonium hydroxide. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was stirred in a dilute ammonium hydroxide solution. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product was filtered off and dried, yielding 2.2 parts of 3-[2-[4-[bis(4-fluorophenyl)methylene]-1-piperidinyl]ethyl]-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one; mp. 108.7° C. (compound 156).

後処理

  1. extractionThe product was extracted with dichloromethane
  2. customThe extract was dried
  3. filtrationfiltered
  4. customevaporated
  5. extractionThe product was extracted with dichloromethane
  6. customThe extract was dried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
  10. filtrationThe product was filtered off
  11. customdried

出典と根拠

ORDレコード
ord-021ad052611a497abeb681eef3bb627c
出典データセット
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04485107

反応ノート

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