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Potassium Carbonate → 5-Cyano-3-amino-2-(2'-ethoxy-5'-fluorobenzoyl)-thieno[2,3-b]pyridine

HRID 450857
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인쇄 미리보기

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HRID 450857 반응식
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([O:9][C:10]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:11]=1[C:12](=[O:15])[CH2:13]Br)[CH3:8].[C:21]([C:23]1[C:24]([SH:31])=[N:25][CH:26]=[C:27]([C:29]#[N:30])[CH:28]=1)#[N:22]>CN(C=O)C.C(OCC)(=O)C>[C:29]([C:27]1[CH:28]=[C:23]2[C:21]([NH2:22])=[C:13]([C:12](=[O:15])[C:11]3[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:10]=3[O:9][CH2:7][CH3:8])[S:31][C:24]2=[N:25][CH:26]=1)#[N:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 587073552-Bromo-1-(2-ethoxy-5-fluorophenyl)ethanoneHCID 178510368HCID 178510368, 화합물

생성물 1

HCID 692826645-Cyano-3-amino-2-(2'-ethoxy-5'-fluorobenzoyl)-thieno[2,3-b]pyridine

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857
Ethyl Acetate
용매

실험 절차

A suspension of potassium carbonate (1.18 g, 8.55 mmol), 2-ethoxy-5-fluorophenacyl bromide (1.34 g, 5.12 mmol) and 3,5-dicyano-2-mercaptopyridine (0.55 g, 3.42 mmol) in dry DMF (8 ml) is stirred at room temperature for 16 h. The resulting mixture is diluted with ethyl acetate and washed with water. Drying over sodium sulfate, filtering, evaporating the solvent and purification of the residue by silicagel column chromatography yields the title compound, having a m.p. of 196° C.

후처리

  1. washwashed with water
  2. dry with materialDrying over sodium sulfate
  3. filtrationfiltering
  4. customevaporating
  5. customthe solvent and purification of the residue by silicagel column chromatography

출처 및 근거

ORD 기록
ord-1d997590e2a64ba6a96a8e4f543e8442
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486996B2

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