1,4-Dioxane → HCID 14152935、化合物

HRID 648487

反応式

HRID 648487 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 14152935HCID 14152935、化合物収率 73%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-be92ae4a412444b888a6a9a14e4eb534
出典データセット
uspto-grants-1988_04
特許番号
US04735942

関連ノート

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