Ethanol → HCID 12852073, 화합물

HRID 1248245노트

반응식

HRID 1248245 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 12852073HCID 12852073, 화합물수율 50%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide촉매HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-aab676c4b055434ead20e113ce209b03
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04522945

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