Pyridine → HCID 58300410, 화합물

HRID 68647노트

반응식

HRID 68647 반응식
[CH2:1]([N:4]([CH2:28][CH2:29][CH3:30])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH2:19][NH:20][CH2:21][C:22]3[N:23]([CH3:27])[CH:24]=[CH:25][N:26]=3)[CH:15]=2)[CH2:10]1)[CH2:2][CH3:3].N1C=CC=CC=1.Cl.[NH:38]1[CH:42]=[CH:41][N:40]=[C:39]1[S:43](Cl)(=[O:45])=[O:44].[OH-].[Na+]>ClCCl>[CH2:28]([N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[CH2:18][CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH2:19][N:20]([CH2:21][C:22]3[N:23]([CH3:27])[CH:24]=[CH:25][N:26]=3)[S:43]([C:39]3[NH:38][CH:42]=[CH:41][N:40]=3)(=[O:45])=[O:44])[CH:15]=2)[CH2:10]1)[CH2:29][CH3:30]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 14798Sodium HydroxideHCID 67163530({2-[4-(dipropylamino)butyl]-1,2,3,4-tetrahydro-6-isoquinolinyl}methyl)[(1-methyl-1H-imidazol-2-yl)methyl]amineHCID 713020781H-Imidazole-2-sulfonyl chloride--hydrogen chloride (1/1)

생성물 1

HCID 58300410HCID 58300410, 화합물수율 90.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a solution of the compound 23-a (100 mg) and pyridine (59 mL) in dichloromethane (3 mL), the compound 36 (74 mg) was added. The reaction mixture was stirred at room temperature for 30 minutes. To the reaction mixture, an aqueous 1N sodium hydroxide solution (15 mL) was added. The aqueous layer was extracted twice with dichloromethane (30 mL). The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated. The residue was purified by silica gel chromatography (ethyl acetate:methanol:triethylamine=10:1:0→10:1:0.5) to obtain the title compound (119 mg) having the following physical properties.

후처리

  1. extractionThe aqueous layer was extracted twice with dichloromethane (30 mL)
  2. washThe combined organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (ethyl acetate:methanol:triethylamine=10:1:0→10:1:0.5)

출처 및 근거

ORD 기록
ord-6e31bd4520b64b39a4d7c0a6b6d349db
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822459B2

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