Guanidine Hydrochloride → HCID 178486745, 화합물

HRID 228977노트

반응식

HRID 228977 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[C:14]2[C:9]([C:10]([O:16][C:17]3[C:18]([CH3:27])=[N:19][C:20]4[C:25]([CH:26]=3)=[CH:24][CH:23]=[CH:22][CH:21]=4)=[CH:11][CH:12]=[N:13]2)=[CH:8][C:7]=1[O:28][CH3:29].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:37][C:38]([NH2:40])=[NH:39].[H-].[Na+]>O.CN(C)C=O>[CH3:29][O:28][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:6]=1[O:5][CH2:4][CH2:3][CH2:2][NH:39][C:38]([NH2:40])=[NH:37])[N:13]=[CH:12][CH:11]=[C:10]2[O:16][C:17]1[C:18]([CH3:27])=[N:19][C:20]2[C:25]([CH:26]=1)=[CH:24][CH:23]=[CH:22][CH:21]=2

참가 물질

7

반응물 4

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 230785037-(3-Chloro-propoxy)-6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinoline2회

생성물 1

HCID 178486745HCID 178486745, 화합물수율 17%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

N,N-Dimethylformamide (1 ml) was added to 7-(3-chloro-propoxy)-6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinoline (compound 375) (40 mg), potassium carbonate (41 mg), and guanidine hydrochloride (28 mg). Sodium hydride (39 mg) was added to the mixture, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution, and the mixture was extracted with n-butanol. The n-butanol layer was washed with water and was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (7 mg, yield 17%).

후처리

  1. extractionthe mixture was extracted with n-butanol
  2. washThe n-butanol layer was washed with water
  3. dry with materialwas then dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-0aeb4c446e4b458e8d067c1e0b1cde6d
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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