Toluene → HCID 12852070, 화합물

HRID 1248246노트

반응식

HRID 1248246 반응식
[NH2:1][C:2]1[CH:26]=[CH:25][CH:24]=[CH:23][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)=[O:5].C(OC(=O)C)(=[O:29])C.C[C:35]1[CH:40]=CC=CC=1>>[F:22][C:19]1[CH:18]=[CH:17][C:16]([C:15]([CH:12]2[CH2:13][CH2:14][N:9]([CH2:8][CH2:7][N:6]3[C:4](=[O:5])[C:3]4[C:2](=[CH:26][CH:25]=[CH:24][CH:23]=4)[N:1]=[C:40]3[CH3:35])[CH2:10][CH2:11]2)=[O:29])=[CH:21][CH:20]=1

참가 물질

4

반응물 3

HCID 1140TolueneHCID 7918Acetic AnhydrideHCID 20278972HCID 20278972, 화합물

생성물 1

HCID 12852070HCID 12852070, 화합물수율 69%

실험 절차

A mixture of 6 parts of 2-amino-N-[2-[4-(4-fluorobenzyl)-1-piperidinyl]ethyl]benzamide, 10 parts of acetic acid anhydride and 108 parts of methylbenzene is stirred and refluxed overnight. The reaction mixture is evaporated and water is added to the oily residue. The whole is alkalized with a dilute sodium hydroxide solution and extracted with trichloromethane. The extract is dried, filtered and evaporated. The oily residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product is filtered off and recrystallized from 2-propanol, yielding 4.4 parts (69%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2-methyl-4(3H)-quinazolinone; mp. 164.9° C.

후처리

  1. temperaturerefluxed overnight
  2. customThe reaction mixture is evaporated
  3. additionwater is added to the oily residue
  4. extractionextracted with trichloromethane
  5. customThe extract is dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe oily residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
  9. filtrationThe product is filtered off
  10. customrecrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-a443e8299cae40e18de1e0158759117c
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04522945

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