Ethanol → HCID 12852073、化合物

HRID 1248245ノート

反応式

HRID 1248245 の反応式
[NH2:1][C:2]1[CH:27]=[CH:26][CH:25]=[CH:24][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15](=[O:23])[C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)=[O:5].C=O.[CH2:30](O)C>[OH-].[Na+].O>[F:22][C:19]1[CH:18]=[CH:17][C:16]([C:15]([CH:12]2[CH2:11][CH2:10][N:9]([CH2:8][CH2:7][N:6]3[C:4](=[O:5])[C:3]4[C:2](=[CH:27][CH:26]=[CH:25][CH:24]=4)[NH:1][CH2:30]3)[CH2:14][CH2:13]2)=[O:23])=[CH:21][CH:20]=1

参加物

6

反応物 3

HCID 702EthanolHCID 712FormaldehydeHCID 30186512-Amino-N-{2-[4-(4-fluorobenzoyl)piperidin-1-yl]ethyl}benzene-1-carboximidic acid

生成物 1

HCID 12852073HCID 12852073、化合物収率 50%

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide触媒HCID 962Water溶媒

実験手順

A mixture of 6.5 parts of 2-amino-N-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]benzamide, 0.5 parts of paraformaldehyde, 3 drops of sodium hydroxide solution 50%, 80 parts of ethanol and 10 parts of water is stirred and refluxed overnight. The reaction mixture is allowed to cool to room temperature while stirring. The precipitated product is filtered off, washed with ethanol and crystallized from 200 parts of ethanol, yielding 3.3 parts (50%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,3-dihydro-4(1H)-quinazolinone; mp. 203.4° C.

後処理

  1. temperaturerefluxed overnight
  2. stirringwhile stirring
  3. filtrationThe precipitated product is filtered off
  4. washwashed with ethanol
  5. customcrystallized from 200 parts of ethanol

出典と根拠

ORDレコード
ord-aab676c4b055434ead20e113ce209b03
出典データセット
uspto-grants-1985_06
特許番号
US04522945

反応ノート

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