p-Toluenesulfonic acid → HCID 20157034、化合物

HRID 986699ノート

反応式

HRID 986699 の反応式
[C:1]([C:4]1[CH:24]=[CH:23][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][C:14]=2[Br:22])=[C:6]([CH2:25][CH2:26][CH3:27])[C:5]=1[OH:28])(=[O:3])[CH3:2].[O:29]1[CH:34]=[CH:33][CH2:32][CH2:31][CH2:30]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)Cl>[C:1]([C:4]1[CH:24]=[CH:23][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:21]=[CH:20][C:16]([C:17]([O:19][CH:30]3[CH2:31][CH2:32][CH2:33][CH2:34][O:29]3)=[O:18])=[CH:15][C:14]=2[Br:22])=[C:6]([CH2:25][CH2:26][CH3:27])[C:5]=1[OH:28])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyranHCID 13338867HCID 13338867、化合物

生成物 1

HCID 20157034HCID 20157034、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In methylene chloride (30 ml) was dissolved 4-[3-(4-acetyl-3-hydroxy-2-propylphenoxy)propoxy]-3-bromobenzoic acid (1.35 g). To the solution were added dihydropyran (0.9 ml) and p-toluene sulfonic acid.monohydrate (5 mg). The mixture was stirred at room temperature for 30 minutes, to which was further added methylene chloride (30 ml). The resulting solution was washed with an aqueous solution of sodium hydrogen carbonate and then with water, followed by drying with sodium sulfate. The solvent was evaporated off, and the residue was purified by means of a silica-gel column chromatography (Developing solvent: chloroform) to give 1.4 g of tetrahydropyranyl 4-[3-(4-acetyl-3-hydroxy-2-propylphenoxy)propoxy]-3-bromobenzoate as colorless oily substance.

後処理

  1. washThe resulting solution was washed with an aqueous solution of sodium hydrogen carbonate
  2. dry with materialby drying with sodium sulfate
  3. customThe solvent was evaporated off
  4. customthe residue was purified by means of a silica-gel column chromatography (Developing solvent: chloroform)

出典と根拠

ORDレコード
ord-8c58465b37b6406998028a61b7e271bf
出典データセット
uspto-grants-1987_12
特許番号
US04714774

反応ノート

読み込み中…