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Guanidine Hydrochloride → HCID 178485148, 화합물

HRID 565041
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HRID 565041 반응식
Cl.[NH2:2][C:3]([NH2:5])=[NH:4].[CH3:6][O-].[Na+].[Cl:9][C:10]1[CH:18]=[C:17]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[N+:26]([O-:28])=[O:27])[CH:16]=[C:15]2[C:11]=1[CH:12]=[C:13]([C:30](OCC)=[O:31])[N:14]2C>CO>[Cl:9][C:10]1[CH:18]=[C:17]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[N+:26]([O-:28])=[O:27])[CH:16]=[C:15]2[C:11]=1[CH:12]=[C:13]([C:30]([N:4]=[C:3]([NH2:5])[NH:2][CH3:6])=[O:31])[NH:14]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5742Guanidine HydrochlorideHCID 10942334Sodium MethoxideHCID 21194137Ethyl 4-chloro-1-methyl-6-(2-nitrophenoxy)-2-indolecarboxylate

생성물 1

HCID 178485148HCID 178485148, 화합물수율 40.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

After 2.87 g (30.0 mmol) of guanidine hydrochloride was added to 25 ml of a methanol solution of 1.62 g (30.0 mmol) of sodium methoxide, the mixture was stirred at room temperature for 30 minutes. The precipitated sodium chloride was filtered off. To the obtained solution was added 0.51 g (1.50 mmol) of ethyl 4-chloro-1-methyl-6-(2-nitrophenoxy)-2-indolecarboxylate. Subsequently methanol was distilled off under reduced pressure. The resulting residue was heated at 130° C. for 5 minutes and then allowed to stand at room temperature for an hour. Thereafter water was poured onto the reaction solution and the mixture was extracted three times with ethyl acetate. The combined extracts were washed with water. After drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was isolated and purified by silica gel column chromatography to give 0.23 g (40.1%) of 4-chloro-1-methyl-6-(2-nitrophenoxy)-2-indoloylguanidine.

후처리

  1. filtrationThe precipitated sodium chloride was filtered off
  2. distillationSubsequently methanol was distilled off under reduced pressure
  3. temperatureThe resulting residue was heated at 130° C. for 5 minutes
  4. waitto stand at room temperature for an hour
  5. additionThereafter water was poured onto the reaction solution
  6. extractionthe mixture was extracted three times with ethyl acetate
  7. washThe combined extracts were washed with water
  8. dry with materialAfter drying over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure
  10. customThe resulting residue was isolated
  11. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e5f8887fe7814dccb5a906b056582338
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06169107A

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