Hydrochloric Acid → Benzoic acid, 4-[(tetrahydro-2H-pyran-2-yl)oxy]-, methyl ester

HRID 621833노트

반응식

HRID 621833 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.Cl.[O:13]1[CH:18]=[CH:17][CH2:16][CH2:15][CH2:14]1>CC(=O)OCC>[O:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 7456MethylparabenHCID 80803,4-dihydro-2H-pyran2회

생성물 1

HCID 11770459Benzoic acid, 4-[(tetrahydro-2H-pyran-2-yl)oxy]-, methyl ester

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of methyl 4-hydroxybenzoate (10 g) in EA (60 ml) containing saturated ethereal HCl (3.5 ml) was treated with dihydropyran (12 ml) and the solution was allowed to stand at room temperature for 24 h. A further quantity of dihydropyran (12 ml) and ethereal HCl (3.5 ml) was added and the solution was left for 17 h. The solvent was evaporated and the residue was dissolved in ER (100 ml) and washed with 2N NaOH solution (2×50 ml), brine (50 ml) and then dried. Evaporation gave a residue which on purification by chromatography using 3:97 ER-toluene as eluant gave the title compound as a white solid (10.2 g), m.p. 58°-62°.

후처리

  1. waitthe solution was left for 17 h
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in ER (100 ml)
  4. washwashed with 2N NaOH solution (2×50 ml), brine (50 ml)
  5. customdried
  6. customEvaporation
  7. customgave a residue which
  8. customon purification by chromatography

출처 및 근거

ORD 기록
ord-132cb0f249214c188fbb6d1184b8e846
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824993

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