Dichloromethane → HCID 67975334, 화합물

HRID 623906노트

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HRID 623906 반응식
C(Cl)Cl.C(O)(=O)C.[C:8]([C:11]1[CH:16]=[CH:15][C:14]([C:17]2[C:18]([CH3:32])=[CH:19][C:20]([O:23][CH2:24][C:25]([CH3:31])([CH3:30])[C:26]([O:28][CH3:29])=[O:27])=[N:21][CH:22]=2)=[CH:13][C:12]=1[F:33])(=[NH:10])[NH2:9].Br[CH2:35][C:36](=O)[CH2:37][CH:38]1[CH2:40][CH2:39]1.C(=O)([O-])[O-].[K+].[K+]>[Cl-].[Na+].O>[CH:38]1([CH2:37][C:36]2[NH:9][C:8]([C:11]3[CH:16]=[CH:15][C:14]([C:17]4[C:18]([CH3:32])=[CH:19][C:20]([O:23][CH2:24][C:25]([CH3:30])([CH3:31])[C:26]([O:28][CH3:29])=[O:27])=[N:21][CH:22]=4)=[CH:13][C:12]=3[F:33])=[N:10][CH:35]=2)[CH2:40][CH2:39]1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 451201162-Propanone, 1-bromo-3-cyclopropyl-HCID 67973349HCID 67973349, 화합물

생성물 1

HCID 67975334HCID 67975334, 화합물수율 79.3%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

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온도
40 °C

실험 절차

A mixture in which methylene chloride (10 mL) and a saturated brine (10 mL) were added to methyl 3-{[5-(4-carbamimidoyl-3-fluorophenyl)-4-methylpyridin-2-yl]oxy}-2,2-dimethylpropanoate acetic acid salt (300 mg), 1-bromo-3-cyclopropylpropan-2-one (190 mg) and potassium carbonate (346 mg) was stirred at 40° C. for 5 hours. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=100:0 to 97:3) to obtain methyl 3-[(5-{4-[5-(cyclopropylmethyl)-1H-imidazol-2-yl]-3-fluorophenyl}-4-methylpyridin-2-yl)oxy]-2,2-dimethylpropanoate (248 mg).

후처리

  1. customThe organic layer was separated
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (chloroform:methanol=100:0 to 97:3)

출처 및 근거

ORD 기록
ord-784334d397d947b4bde7dd1d0e29ee8a
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302996B2

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