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

HRID 567741ノート

反応式

HRID 567741 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 178486819HCID 178486819、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.).

後処理

  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)

出典と根拠

ORDレコード
ord-ffc2370ea3d14ff3891a234d8a9eb68d
出典データセット
uspto-grants-2001_01
特許番号
US06180632B2

反応ノート

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