Dimethylhydantoin → Nilutamide

HRID 374123

反応式

HRID 374123 の反応式
COCCOCCOCCOC.[N+:13]([C:16]1[CH:21]=[CH:20][C:19](Cl)=[CH:18][C:17]=1[C:23]([F:26])([F:25])[F:24])([O-:15])=[O:14].[CH3:27][C:28]1([CH3:35])[NH:32][C:31](=[O:33])[NH:30][C:29]1=[O:34]>>[F:24][C:23]([F:26])([F:25])[C:17]1[CH:18]=[C:19]([N:30]2[C:29](=[O:34])[C:28]([CH3:35])([CH3:27])[NH:32][C:31]2=[O:33])[CH:20]=[CH:21][C:16]=1[N+:13]([O-:15])=[O:14]

参加物

4

反応物 3

HCID 6491DimethylhydantoinHCID 8189TriglymeHCID 670525-Chloro-2-nitrobenzotrifluoride

生成物 1

HCID 4493Nilutamide収率 30%

反応条件

温度
20 °C

実験手順

The following were introduced into 282 ml of triglyme: 112.8 grams of 2-nitro-5-chloro-trifluoromethylbenzene, 64.1 grams of 5,5-dimethyl-hydantoin and 33.5 grams of cuprous oxide. The mixture was heated to about 215° C.±5° C. for 4 hours, then cooled to 20° C. and filtered. The triglyme solution was recovered and a 22 Be ammonia solution (1V), toluene (1V) and demineralized water (4V) were added to the solution of triglyme (1V). The solution was stirred at 20° C. for 15 minutes, then cooled to about -10° C. and stirred again at -10° C. After washing and drying, 47.6 grams of the desired product were obtained.

後処理

  1. temperatureThe mixture was heated to about 215° C.±5° C. for 4 hours
  2. filtrationfiltered
  3. customThe triglyme solution was recovered
  4. additiona 22 Be ammonia solution (1V), toluene (1V) and demineralized water (4V) were added to the solution of triglyme (1V)
  5. temperaturecooled to about -10° C.
  6. stirringstirred again at -10° C
  7. washAfter washing
  8. customdrying

出典と根拠

ORDレコード
ord-e1a261677b474525b612c97fa3ced3ef
出典データセット
uspto-grants-1992_11
特許番号
US05166358

関連ノート

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