p-Toluenesulfonic acid → HCID 20157034, 화합물

HRID 986699노트

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HRID 986699 반응식
[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]

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyranHCID 13338867HCID 13338867, 화합물

생성물 1

HCID 20157034HCID 20157034, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8c58465b37b6406998028a61b7e271bf
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04714774

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