HCID 22018329、化合物 → HCID 178458193、化合物

HRID 1368537ノート

反応式

HRID 1368537 の反応式
[CH:1]([O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[CH:11]=[C:10]([C:15]([C:20]1[N:21]=[CH:22][N:23](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:24]=1)([OH:19])[CH:16]([CH3:18])[CH3:17])[CH:9]=[CH:8]2)([CH3:3])[CH3:2]>C(O)(=O)C.O>[CH:1]([O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[CH:11]=[C:10]([C:15]([C:20]1[N:21]=[CH:22][NH:23][CH:24]=1)([OH:19])[CH:16]([CH3:18])[CH3:17])[CH:9]=[CH:8]2)([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 22018329HCID 22018329、化合物

生成物 1

HCID 178458193HCID 178458193、化合物収率 67.8%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

1-(6-Isopropoxynaphthalen-2-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (0.438 g) was dissolved in a mixture of acetic acid (20 ml) and water (0.5 ml), and the solution was stirred at 50° C. for 18 h. The solvent was evaporated, and to the mixture was added ethyl acetate. The mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution. The organic layer was dried and concentrated. The obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=40:1→20:1) to give the titled compound (0.170 g) as an amorphous product.

後処理

  1. customThe solvent was evaporated
  2. additionto the mixture was added ethyl acetate
  3. washThe mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution
  4. customThe organic layer was dried
  5. concentrationconcentrated
  6. customThe obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=40:1→20:1)

出典と根拠

ORDレコード
ord-c51d8eb8d17e4290ab134e3548f294cd
出典データセット
uspto-grants-2003_06
特許番号
US06573289B1

反応ノート

読み込み中…