Methanol → 4-Methoxyquinoline

HRID 2193100

反応式

HRID 2193100 の反応式
CO.[OH:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[CH:6][CH:5]=1.[CH:14](N(C(C)C)CC)(C)C.C[Si](C=[N+]=[N-])(C)C.CCCCCC>C(#N)C>[CH3:14][O:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 887MethanolHCID 81531DiisopropylethylamineHCID 86587183Trimethylsilyldiazomethane hexaneHCID 178516385quinolin-4-ol

生成物 1

HCID 5219384-Methoxyquinoline

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To 15 mL of methanol containing 4.02 g of 4-hydroxyquinoline and 130 mL of an acetonitrile solution, 5.01 g of diisopropylethylamine and 19.4 mL of a 2.0 mol/L trimethylsilyldiazomethane/hexane solution were added at room temperature, and the mixture was stirred for 13 hours, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [silica gel; Chromatorex-NH, manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate 2:1] to obtain 1.79 g of a yellow oily substance, 4-methoxyquinoline.

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe residue thus obtained
  3. customwas purified by silica gel column chromatography [silica gel; Chromatorex-NH, manufactured by Fuji Silysia Chemical Ltd., eluent; hexane:ethyl acetate 2:1]

出典と根拠

ORDレコード
ord-b4f3a044719c4fe6b161a71daf6afef5
出典データセット
uspto-grants-2012_12
特許番号
US08329694B2

関連ノート

読み込み中…