1,4-Dioxane → HCID 14152935, 화합물

HRID 648487

반응식

HRID 648487 반응식
C1(O[C:8](=[O:30])[NH:9][C:10]2[CH:15]=[CH:14][C:13]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)=[CH:12][CH:11]=2)C=CC=CC=1.C([O:33][C:34](=O)[CH2:35][NH:36][CH:37]([CH3:39])[CH3:38])C.O1CCOCC1>CN(C)C1C=CN=CC=1.O>[CH3:29][O:28][C:25]1[CH:26]=[CH:27][C:22]([N:19]2[CH2:20][CH2:21][N:16]([C:13]3[CH:12]=[CH:11][C:10]([N:9]4[C:34](=[O:33])[CH2:35][N:36]([CH:37]([CH3:39])[CH3:38])[C:8]4=[O:30])=[CH:15][CH:14]=3)[CH2:17][CH2:18]2)=[CH:23][CH:24]=1

참가 물질

6

반응물 3

HCID 312751,4-DioxaneHCID 351625Ethyl 2-((propan-2-yl)amino)acetateHCID 981607Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate

생성물 1

HCID 14152935HCID 14152935, 화합물수율 73%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매

실험 절차

A mixture of 5 parts of phenyl[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate, 3 parts of ethyl[(1-methylethyl)amino]acetate, 1 part of N,N-dimethyl-4-pyridinamine and 100 parts of 1,4-dioxane was stirred and refluxed overnight. The warm solution was saturated with water and allowed to cool. The solution was poured onto water and extracted with trichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The filtrate was evaporated and the residue was crystallized from methylbenzene, yielding 3.7 parts (73%) of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-1-(1-methylethyl)-2,4-imidazolidinedione; mp. 193.7° C. (38).

후처리

  1. temperaturerefluxed overnight
  2. temperatureto cool
  3. additionThe solution was poured onto water
  4. extractionextracted with trichloromethane
  5. washThe extract was washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. filtrationThe residue was purified by filtration over silica gel using
  10. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
  11. customThe filtrate was evaporated
  12. customthe residue was crystallized from methylbenzene

출처 및 근거

ORD 기록
ord-be92ae4a412444b888a6a9a14e4eb534
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735942

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