HCID 11379002, 화합물 → HCID 178513055, 화합물

HRID 898815노트

반응식

HRID 898815 반응식
C[O:2][C:3]([C:5]1[O:6][C:7]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:8][CH:9]=1)=O.CS(O)(=O)=O.FC1C=CC=CC=1C1OC(C([NH:36][C:37]([NH2:39])=[NH:38])=O)=CC=1>CO.[Cl-].[Na+].O>[F:16][C:13]1[CH:14]=[CH:15][C:10]([C:7]2[O:6][C:5]([C:3]([NH:38][C:37]([NH2:39])=[NH:36])=[O:2])=[CH:9][CH:8]=2)=[CH:11][CH:12]=1

참가 물질

5

반응물 2

HCID 11379002HCID 11379002, 화합물HCID 178505355HCID 178505355, 화합물

생성물 1

HCID 178513055HCID 178513055, 화합물수율 51.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 57417360Sodium chloride; water용매

실험 절차

5-(4-fluorophenyl)furan-2-carboxylic acid methyl ester (220 mg, 1.0 mmol) was dissolved in methanol (4 ml), to which 2 M guanidine solution (3.0 ml, 6.0 mmol) prepared in Example 1 was added, and the mixture was heated at reflux for 12 hours. After completion of the reaction, the solution was added with saturated brine (20 ml) and extracted with ethyl acetate (30 ml×3). The organic layer was washed with 10% brine, dried over anhydrous magnesium sulfate (MgSO4), and concentrated in vacuo. The residue was purified by silica gel column chromatography (5% methanol/dichloromethane), to give 127 mg of a title compound (yield: 51%).

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 12 hours
  4. customAfter completion of the reaction
  5. extractionextracted with ethyl acetate (30 ml×3)
  6. washThe organic layer was washed with 10% brine
  7. dry with materialdried over anhydrous magnesium sulfate (MgSO4)
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by silica gel column chromatography (5% methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-df06d6e6b2ca4bd898935427db93b9e9
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07351843B2

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