2-(6,7-Dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-one → HCID 178486819, 화합물

HRID 1859504

반응식

HRID 1859504 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[C:8]([N:15]1C(=O)[CH:19]3[CH2:22][CH2:23][CH:16]1[CH2:17][CH2:18]3)[CH:7]=[N:6]2.[CH3:24][O-:25].[Na+].[CH3:27][OH:28]>CO>[CH3:24][O:25][C:27]([C@H:19]1[CH2:18][CH2:17][C@H:16]([NH:15][C:8]2[CH:7]=[N:6][C:5]3[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=3)[N:9]=2)[CH2:23][CH2:22]1)=[O:28]

참가 물질

4

반응물 2

HCID 225731612-(6,7-Dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-oneHCID 23694274Sodium methanolate methanol

생성물 1

HCID 178486819HCID 178486819, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-(6,7-dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-one (100 mg, 0.32 mmole) in 10 mL of methanol is added a freshly prepared NaOMe/methanol solution (54 mg, 1 mmole) and the mixture is stirred at ROOM TEMPERATURE for 0.5 hour before concentrated. Methylene chloride is used to extract and then dried with magnesium sulfate. The residue after filtration and concentration is chromatographed on silica gel (40% ethyl acetate) to give 85 mg (77%) of cis/trans-4-(6,7-dimethoxy-quinoxalin-2-ylamino)-cyclohexanecarboxylic acid methyl ester as a light yellow solid (m.p. 68-80° C.).

후처리

  1. concentrationbefore concentrated
  2. extractionto extract
  3. dry with materialdried with magnesium sulfate
  4. filtrationThe residue after filtration and concentration
  5. customis chromatographed on silica gel (40% ethyl acetate)

출처 및 근거

ORD 기록
ord-e05b0f83ce46413894c68559a015a58f
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06528526B1

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