2-Chlorophenol → 8-Chloro-4-(2-chlorophenoxy)quinoline

HRID 1885530ノート

反応式

HRID 1885530 の反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([Cl:12])[CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][CH:3]=1.[Cl:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[OH:20]>C(OCC)(=O)C>[Cl:12][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:6]=1[N:5]=[CH:4][CH:3]=[C:2]2[O:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[Cl:13]

参加物

4

反応物 2

HCID 72452-ChlorophenolHCID 889734,8-Dichloroquinoline2 回

生成物 1

HCID 1641768-Chloro-4-(2-chlorophenoxy)quinoline

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
160 °C

実験手順

A mixture of 2.0 g of 4,8-dichloroquinoline and 2.6 g of 2-chlorophenol was heated to 160° C. and stirred. Progress of the reaction was monitored by TLC. When no 4,8-dichloroquinoline remained, the reaction mixture was diluted with ethyl acetate, and washed with base to remove most of the excess phenol. To remove phenol remaining after washing, the product was purified using HPLC. Fractions containing product were combined, and solvent was removed using reduced pressure. The oily product crystallized. Yield: 1.36 g (46%). M.P. 56°-58° C.

後処理

  1. washwashed with base
  2. customto remove most of the excess phenol
  3. customTo remove phenol remaining
  4. washafter washing
  5. customthe product was purified
  6. additionFractions containing product
  7. customsolvent was removed
  8. customThe oily product crystallized

出典と根拠

ORDレコード
ord-417cddfe79ff4dbfb8309536995f387b
出典データセット
uspto-grants-1992_09
特許番号
US05145843

反応ノート

読み込み中…