Ethylene Glycol → HCID 86643578, 화합물

HRID 1848962노트

반응식

HRID 1848962 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[C:5](I)=[CH:4][N:3]=1.[C:10]1([SH:16])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)CO.C(=O)([O-])[O-].[K+].[K+]>[Cu]I.C(O)(C)C>[Cl:1][C:2]1[C:7]([S:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1

참가 물질

7

반응물 4

HCID 174Ethylene GlycolHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 454803662-Chloro-5-iodopyridin-4-amine

생성물 1

HCID 86643578HCID 86643578, 화합물수율 97%

시약·촉매·용매 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 3776Isopropanol용매

실험 절차

To a 250 mL round flask was added 2-chloro-5-iodo-4-aminopyridine (5.0 g, 19.6 mmol), thiophenol (2.16 g, 19.6 mmol), CuI (0.187 g, 0.98 mmol), ethylene glycol (2.5 g, 39 mmol), potassium carbonate (5.4 g, 39 mmol), and 150 mL of isopropanol. The reaction was heated to reflux and stirred under a nitrogen atmosphere for 24 h. After cooling, the mixture was purified by a silica gel column. Yield (97%) of 2-chloro-3-phenylthio-4-aminopyridine was 4.5 g.

후처리

  1. temperatureThe reaction was heated
  2. temperatureto reflux
  3. temperatureAfter cooling
  4. customthe mixture was purified by a silica gel column

출처 및 근거

ORD 기록
ord-7bb80aa41eaf411fa931a8b21c79ebf4
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952363B2

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