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

HRID 634548ノート

反応式

HRID 634548 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3a7dde98dbdd4dc79319995cc86ee9a1
出典データセット
uspto-grants-2016_04
特許番号
US09324949B2

反応ノート

読み込み中…