Potassium Acetate → HCID 22397176、化合物

HRID 1070644ノート

反応式

HRID 1070644 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[C:10](Cl)[N:11]=[C:12]([CH2:17][N:18]3[CH2:23][CH2:22][O:21][CH2:20][CH2:19]3)[CH:13]=2)[N:8]([CH3:25])[CH:7]=1)=[O:5])[CH3:2].C([O-])(=O)C.[K+]>C(O)(C)C.[Pd]>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][N:11]=[C:12]([CH2:17][N:18]3[CH2:19][CH2:20][O:21][CH2:22][CH2:23]3)[CH:13]=2)[N:8]([CH3:25])[CH:7]=1)=[O:5])[CH3:2]

参加物

5

反応物 2

HCID 517044Potassium AcetateHCID 22397142HCID 22397142、化合物

生成物 1

HCID 22397176HCID 22397176、化合物収率 711.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 3776Isopropanol溶媒

実験手順

A mixture of ethyl-8-chloro-1-methyl-6-(4-morpholinylmethyl)-4-oxo-1,4-dihydro-[1,7]naphthyridine-3-carboxylate (Preparation 45, 0.090 g), potassium acetate (0.015 g) and 10% Pd/C (20 mg) in isopropyl alcohol is hydrogenated (balloon) for 18 hours. The mixture is filtered through celite and the filter cake washed with MeOH. The solvent is evaporated and the crude solid chromatographed with CH2Cl2\CH3OH\TEA (90\9\1) to obtain 0.58 g (70%) of the title compound as an off-white solid. Physical characteristics: MS (ESI+) m/z 332 (M+H).

後処理

  1. customfor 18 hours
  2. filtrationThe mixture is filtered through celite
  3. washthe filter cake washed with MeOH
  4. customThe solvent is evaporated
  5. customthe crude solid chromatographed with CH2Cl2\CH3OH\TEA (90\9\1)

出典と根拠

ORDレコード
ord-0bb9612b346c4e9890b602e1185d6e83
出典データセット
uspto-grants-2005_06
特許番号
US06903097B2

反応ノート

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