Water → 8-Chlorobenzofuro[3,2-c]pyridine

HRID 634548노트

반응식

HRID 634548 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:15]C)=[C:6]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:13]=2N)[CH:7]=1.C1COCC1.O>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:15][C:13]3[CH:12]=[CH:11][N:10]=[CH:9][C:8]=3[C:6]=2[CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 8028TetrahydrofuranHCID 509670043-(5-Chloro-2-methoxyphenyl)pyridin-4-amine

생성물 1

HCID 441784398-Chlorobenzofuro[3,2-c]pyridine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

3-(5-chloro-2-methoxyphenyl)pyridin-4-amine (2 g, 8.5 mmol) was dissolved in 25 mL of acetic acid and 10 mL of THF at −10° C. To the solution t-butyl nitrile (2 ml, 17 mmol) was dropwisely added. The mixture was warmed to room temperature overnight. Water was added to the reaction mixture and was extracted by dichloromethane, the organic layer was then dried by MgSO4 and concentrated. The residue was then purified by column chromatography using THF:hexane (1:3, v/v) as the eluent. 0.8 g (46%) of product was collected as the product.

후처리

  1. customat −10° C
  2. extractionwas extracted by dichloromethane
  3. dry with materialthe organic layer was then dried by MgSO4
  4. concentrationconcentrated
  5. customThe residue was then purified by column chromatography
  6. custom0.8 g (46%) of product was collected as the product

출처 및 근거

ORD 기록
ord-3a7dde98dbdd4dc79319995cc86ee9a1
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09324949B2

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