Ethanol → Ethyl(E)-3-[2-amino-4-(4-aminophenoxy)-3-pyridyl]-propenoate

HRID 1010186노트

반응식

HRID 1010186 반응식
[NH2:1][C:2]1[C:7](/[CH:8]=[CH:9]/[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:6]([O:15][C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][CH:17]=2)[CH:5]=[CH:4][N:3]=1.[Cl-].[NH4+].CN(C)C=O.C(O)C>[Fe].O>[NH2:1][C:2]1[C:7](/[CH:8]=[CH:9]/[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:6]([O:15][C:16]2[CH:17]=[CH:18][C:19]([NH2:22])=[CH:20][CH:21]=2)[CH:5]=[CH:4][N:3]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 58931221Ethyl(E)-3-[2-amino-4-(4-nitrophenoxy)-3-pyridyl]-2-propenoate

생성물 1

HCID 58931285Ethyl(E)-3-[2-amino-4-(4-aminophenoxy)-3-pyridyl]-propenoate

시약·촉매·용매 2

HCID 23925Iron촉매HCID 962Water용매

실험 절차

Ethyl (E)-3-[2-amino-4-(4-nitrophenoxy)-3-pyridyl]-2-propenoate (350 mg), iron powder (700 mg), ammonium chloride (1.4 g), dimethylformamide (7 ml), ethanol (2 ml) and water (2 ml) were stirred at 100° C. for 20 minutes. The mixture was filtered with celite, and then water and ethyl acetate were added for extraction. The organic layer was washed 5 times with aqueous ammonium chloride solution and then dried over magnesium sulfate. The drying agent was filtered off and the solvent was distilled off under reduced pressure to obtain 230 mg of the target substance as a light yellow solid.

후처리

  1. filtrationThe mixture was filtered with celite
  2. additionwater and ethyl acetate were added for extraction
  3. washThe organic layer was washed 5 times with aqueous ammonium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe drying agent was filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. customto obtain 230 mg of the target substance as a light yellow solid

출처 및 근거

ORD 기록
ord-f01ae8034cb246f2b03415942e9b1283
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973160B2

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