Potassium Carbonate → HCID 117667312, 화합물

HRID 712666노트

반응식

HRID 712666 반응식
[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

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 117667367HCID 117667367, 화합물

생성물 1

HCID 117667312HCID 117667312, 화합물수율 40.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-480fadfbceec4e2086afe51f5b3523dc
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181272B2

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