Ibuprofen, (+-)- → Ibuprofen, Sodium Salt

HRID 1288099

반응식

HRID 1288099 반응식
C(OC(=C(C1C=CC(CC(C)C)=CC=1)C)C#N)(=O)C.[Cl-].[Na+:21].[OH-].[Na+].S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+].[CH2:36]([C:40]1[CH:45]=[CH:44][C:43]([CH:46]([CH3:50])[C:47]([OH:49])=[O:48])=[CH:42][CH:41]=1)[CH:37]([CH3:39])[CH3:38].[Na]>COCCOCCOC.O>[CH2:36]([C:40]1[CH:41]=[CH:42][C:43]([CH:46]([CH3:50])[C:47]([O-:49])=[O:48])=[CH:44][CH:45]=1)[CH:37]([CH3:39])[CH3:38].[Na+:21]

참가 물질

9

반응물 6

HCID 3672Ibuprofen, (+-)-HCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 62648Ammonium PersulfateHCID 5360545SodiumHCID 537773242-(Acetyloxy)-3-[4-(2-methylpropyl)phenyl]-2-butenenitrile

생성물 1

HCID 5338317Ibuprofen, Sodium Salt

시약·촉매·용매 2

HCID 962Water용매HCID 8150Diglyme용매

반응 조건

온도
25 °C

실험 절차

A portion of the enol-acetate solution (V) from A above, (55.41 g. representing 49.3 mmole of enol-acetate) was placed in a 250 ml. 1 necked flask and stirred magnetically while 10 ml. of saturated sodium chloride solution and 16.0 g. of 50 percent sodium hydroxide (200 meq.) were added. The mixture was stirred and allowed to cool to 25° C. and the ammonium persulfate [(NH4)2S2O8 ] (12.5 g.; 55 meq.) in 16 ml. of water were added over 10 minutes. After stirring overnight, 10 ml. of diglyme was added and the pH was adjusted from 9 to 13. The mixture was slowly cooled to 0° C. with seeding with crystals of 2-(4'-isobutylphenyl)propionic acid, sodium salt and held at 0° C. for 3 hours to form solid sodium 2-(4'-isobutylphenyl)propionate (VI) as a crystalline precipitate.

후처리

  1. stirringThe mixture was stirred
  2. stirringAfter stirring overnight
  3. temperatureThe mixture was slowly cooled to 0° C.

출처 및 근거

ORD 기록
ord-873fe138cbda45109326e511d61118a2
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03987094

연결된 노트

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