Hydrochloric Acid → 2-Methyl-1-{7-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethoxy]-1H-indol-3-yl}propan-2-amine

HRID 1351985노트

반응식

HRID 1351985 반응식
[CH3:1][C:2]([NH:25]C(=O)OC(C)(C)C)([CH3:24])[CH2:3][C:4]1[C:12]2[C:7](=[C:8]([O:13][C@@H:14]([CH3:23])[C:15]([N:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[O:16])[CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1.Cl.C(=O)([O-])O.[Na+]>C(Cl)Cl.O1CCOCC1>[CH3:1][C:2]([NH2:25])([CH3:24])[CH2:3][C:4]1[C:12]2[C:7](=[C:8]([O:13][C@@H:14]([CH3:23])[C:15]([N:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[O:16])[CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 86604034tert-butyl (1,1-dimethyl-2-{7-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethoxy]-1H-indol-3-yl}ethyl)carbamate

생성물 1

HCID 694581352-Methyl-1-{7-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethoxy]-1H-indol-3-yl}propan-2-amine수율 53.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of tert-butyl (1,1-dimethyl-2-{7-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethoxy]-1H-indol-3-yl}ethyl)carbamate (166 mg, 0.373 mmol) in methylene chloride (2 mL) is added a 4N hydrogen chloride solution in dioxane (0.5 mL), and the mixture is stirred at room temperature for 3 hours. The reaction solution is poured into a saturated aqueous sodium hydrogen carbonate solution, and the mixture is extracted with chloroform. The organic layer is dried over anhydrous magnesium sulfate, and the solvent is evaporated. The obtained crude product is purified by silica gel column chromatography (a saturated ammonia solution in chloroform ) a saturated ammonia solution in chloroform-methanol=50:1) to give the title compound (68.4 mg, yield: 53%).

후처리

  1. extractionthe mixture is extracted with chloroform
  2. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
  3. customthe solvent is evaporated
  4. customThe obtained crude product
  5. customis purified by silica gel column chromatography (a saturated ammonia solution in chloroform ) a saturated ammonia solution in chloroform-methanol=50:1)

출처 및 근거

ORD 기록
ord-dd418bb49995460480958d08c9df89a4
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217724B2

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