Water → HCID 20148855, 화합물

HRID 569256노트

반응식

HRID 569256 반응식
[OH-:1].[Na+].[CH2:3]([N:10]1[C:14](=O)[CH2:13][CH:12]([CH2:16][C:17]#N)[CH:11]1[C:19]1[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][C:20]=1[Cl:26])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[OH2:27]>>[CH2:3]([N:10]1[CH2:14][CH2:13][CH:12]([CH2:16][C:17]([OH:27])=[O:1])[CH:11]1[C:19]1[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][C:20]=1[Cl:26])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

4

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 20148837HCID 20148837, 화합물

생성물 1

HCID 20148855HCID 20148855, 화합물

실험 절차

To 90 ml of water containing 10 g of sodium hydroxide was added 5.0 g of 1-benzyl-3-cyanomethyl-2-(2,6-dichlorophenyl)pyrrolidin-5-one. The reaction was refluxed 5 hours, cooled, and filtered. Extraction of the aqueous phase with ether followed by addition of ice and acidification with concentrated hydrochloric acid gave a solid which was then triturated with ether to yield beige crystals. Vacuum drying (0.1 Torr) under refluxing toluene for 15 hours followed by recrystallization from ethanol provided upon drying 1.50 g of colorless crystals, m.p. 186°-188°.

후처리

  1. temperatureThe reaction was refluxed 5 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. extractionExtraction of the aqueous phase with ether
  5. additionfollowed by addition of ice and acidification with concentrated hydrochloric acid
  6. customgave a solid which
  7. customwas then triturated with ether
  8. customto yield beige crystals
  9. customVacuum drying (0.1 Torr) under refluxing toluene for 15 hours
  10. customfollowed by recrystallization from ethanol
  11. customprovided
  12. dry with materialupon drying 1.50 g of colorless crystals, m.p. 186°-188°

출처 및 근거

ORD 기록
ord-3f09fc41733647329d35bb4d5935a460
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731457

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