Formic Acid → 3-(3,4-Dimethoxyphenyl)propionic acid

HRID 36408

반응식

HRID 36408 반응식
CC1(C)[O:9][C:7](=[O:8])[CH2:6][C:4](=O)O1.C(=O)[C:12]1[CH:21]=[CH:20][C:17]([O:18][CH3:19])=[C:14]([O:15][CH3:16])[CH:13]=1.C(O)=O.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH3:16][O:15][C:14]1[CH:13]=[C:12]([CH2:4][CH2:6][C:7]([OH:9])=[O:8])[CH:21]=[CH:20][C:17]=1[O:18][CH3:19]

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 8419VeratraldehydeHCID 8471TriethylamineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

생성물 1

HCID 750193-(3,4-Dimethoxyphenyl)propionic acid

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
100 °C

실험 절차

After weighing 7.2 g (0.05 mol) of Meldrum's acid and 8.3 g (0.05 mol) of veratraldehyde to 50 ml of the mixture of formic acid and triethylamine prepared according to Example 1, the reaction mixture was heated to 100° C. during 1 hour and maintained at the same temperature for further 1 hour. Then the excess of formic acid and triethylamine was distilled off under reduced pressure of 2 kPa to give a distillate of 40 ml volume. The distillation residue was dissolved in 100 ml of chloroform and extracted with 50 ml of 1N sodium hydroxide solution. The chloroform phase was extracted with 2×100 ml of 1N sodium hydroxide solution. Thereafter Example 1 was followed to give a yield of 8.6 g (81.8%), m.p.: 96°-97° C.

후처리

  1. customprepared
  2. temperaturemaintained at the same temperature for further 1 hour
  3. distillationThen the excess of formic acid and triethylamine was distilled off under reduced pressure of 2 kPa
  4. customto give a distillate of 40 ml volume
  5. extractionextracted with 50 ml of 1N sodium hydroxide solution
  6. extractionThe chloroform phase was extracted with 2×100 ml of 1N sodium hydroxide solution
  7. customto give a yield of 8.6 g (81.8%), m.p.: 96°-97° C.

출처 및 근거

ORD 기록
ord-da75330b567a43748d4eea55b9536987
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05414108

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