Water → HCID 178480057, 화합물

HRID 1885250노트

반응식

HRID 1885250 반응식
Cl.[NH2:2][C:3]([NH2:5])=[NH:4].[CH3:6][C:7]([C:10]1[CH:11]=[C:12]([CH:21]=[C:22]2[N:26]([CH3:27])[C:25](SC)=[N:24][C:23]2=[O:30])[CH:13]=[C:14]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:15]=1[OH:16])([CH3:9])[CH3:8].CC(C)([O-])C.[K+].O>C(O)C>[CH3:6][C:7]([C:10]1[CH:11]=[C:12]([CH:21]=[C:22]2[N:26]([CH3:27])[C:25]([NH:4][C:3]([NH2:5])=[NH:2])=[N:24][C:23]2=[O:30])[CH:13]=[C:14]([C:17]([CH3:20])([CH3:19])[CH3:18])[C:15]=1[OH:16])([CH3:9])[CH3:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 5742Guanidine HydrochlorideHCID 23665647Potassium tert-butoxideHCID 54334135HCID 54334135, 화합물

생성물 1

HCID 178480057HCID 178480057, 화합물수율 20.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Guanidine hydrochloride (1.7 g, 18 mmoles) is added to a mixture of 5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene)-1,5-dihydro-1-methyl-2-(methylthio)-4-H-imidazole-4-one (3.0 g, 8 mmoles) and potassium tert-butoxide (1.5 g, 13 mmoles) in ethanol (50 mL), and stirred and heated to reflux under an inert atmosphere. After 24 hours the mixture is allowed to cool, and is poured into water (300 mL) and stirred. After half an hour the product is filtered off, rinsed three times with water and dried. Recrystallization from ethanol/DMF gave pure 5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene)-4,5-dihydro-1-methyl-4-oxo-1H-imidazol-2-yl-guanidine (0.6 g), mp 288°-290° C. (dec).

후처리

  1. temperatureheated
  2. temperatureto reflux under an inert atmosphere
  3. temperatureto cool
  4. stirringstirred
  5. filtrationAfter half an hour the product is filtered off
  6. washrinsed three times with water
  7. customdried
  8. customRecrystallization from ethanol/DMF

출처 및 근거

ORD 기록
ord-0d64d5e2a42047b48ccb84de5c665ce7
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05143928

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