Ethanol → HCID 178480057, 화합물

HRID 1885252노트

반응식

HRID 1885252 반응식
[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]2[N:21]([CH3:22])[C:20](SC)=[N:19][C:18]2=[O:25])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])[CH3:3].Cl.[NH2:27][C:28]([NH2:30])=[NH:29].C(O)C.CC(C)([O-])C.[K+]>O>[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]2[N:21]([CH3:22])[C:20]([NH:29][C:28]([NH2:30])=[NH:27])=[N:19][C:18]2=[O:25])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])[CH3:3]

참가 물질

6

반응물 4

HCID 702EthanolHCID 5742Guanidine HydrochlorideHCID 23665647Potassium tert-butoxideHCID 54334135HCID 54334135, 화합물

생성물 1

HCID 178480057HCID 178480057, 화합물수율 47.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5-[[3,5-bis(1,1-dimethylethyl)-4hydroxyphenyl]methylene]-1,5-dihydro-1-methyl-2-(methylthio)-4H-imidazol-4-one (3.0 g, 8 mmoles), guanidine hydrochloride (1.7 g, 18 mmoles) and 50 mL of ethanol is treated with potassium t-butoxide (1.5 g, 13 mmoles) and heated under reflux for 20 hours, then stirred into 400 mL of water. The precipitate is filtered off, rinsed with water, dried, and recrystallized from acetone to afford the product (1.4 g), mp 286°-287° C. (dec). A sample recrystallized from DMF/EtOH was analytically pure which is N-[5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-4,5-dihydro-1-methyl-4-oxo-1H-imidazol-2-yl]guanidine, mp 288°-290° C. (dec).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 20 hours
  3. filtrationThe precipitate is filtered off
  4. washrinsed with water
  5. customdried
  6. customrecrystallized from acetone

출처 및 근거

ORD 기록
ord-11db9de4a0334c2db1acf0e3cb9a058e
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05143928

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