Potassium Carbonate → HCID 117667312、化合物

HRID 712666ノート

反応式

HRID 712666 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:16]=[C:17]3[C:22](=[N:23][CH:24]=2)[N:21]([C:25]([NH:27]C(=O)C2C=CC=CC=2)=[O:26])[CH2:20][CH2:19][CH2:18]3)[CH:12]=[N:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+]>CCO>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:16]=[C:17]3[C:22](=[N:23][CH:24]=2)[N:21]([C:25]([NH2:27])=[O:26])[CH2:20][CH2:19][CH2:18]3)[CH:12]=[N:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 117667367HCID 117667367、化合物

生成物 1

HCID 117667312HCID 117667312、化合物収率 40.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a mixture of N-[6-(5-benzyloxy-pyridin-3-yl)-3,4-dihydro-2H-[1,8]naphthyridine-1-carbonyl]-benzamide (620 mg, 1.3 mmol) in EtOH (23 ml) is added potassium carbonate (276 mg, 2.0 mmol). The resultant mixture is heated at reflux for 15 min. After cooling to rt, the solid is removed by filtration and the filtrate is concentrated under vacuum. The residue is dissolved in DCM, washed with water and brine, and is dried (Na2SO4). The solvent is evaporated and the crude product is purified by silica gel column to afford 6-(5-benzyloxy-pyridin-3-yl)-3,4-dihydro-2H-[1,8]naphthyridine-1-carboxylic acid amide (188 mg).

後処理

  1. temperatureat reflux for 15 min
  2. customthe solid is removed by filtration
  3. concentrationthe filtrate is concentrated under vacuum
  4. dissolutionThe residue is dissolved in DCM
  5. washwashed with water and brine
  6. dry with materialis dried (Na2SO4)
  7. customThe solvent is evaporated
  8. customthe crude product is purified by silica gel column

出典と根拠

ORDレコード
ord-480fadfbceec4e2086afe51f5b3523dc
出典データセット
uspto-grants-2015_11
特許番号
US09181272B2

反応ノート

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