3-Pyridinemethanol → p-Isobutylphenylacetic acid-3-pyridylmethyl ester

HRID 26462

반응식

HRID 26462 반응식
[Na].[OH:2][CH2:3][C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1.C[O:11][C:12](=O)[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:16][CH:15]=1>O>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([CH2:3][O:2][C:12](=[O:11])[CH2:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][CH:21]([CH3:22])[CH3:23])=[CH:16][CH:15]=2)[CH:5]=1

참가 물질

5

반응물 3

HCID 75103-PyridinemethanolHCID 5360545SodiumHCID 10987436Methyl 2-(4-isobutylphenyl)acetate

생성물 1

HCID 21323306p-Isobutylphenylacetic acid-3-pyridylmethyl ester

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 0.05 g of sodium and 8 ml of 3-hydroxymethylpyridine was heated at 65°-70° C. for 10 hours. To this mixture was added 2.1 g of p-isobutylphenylacetic acid methyl ester, and the whole was heated at 95°-100° C. for 8 hours. After the reaction was complete, 100 ml of water was added. The resulting mixture was extracted with ether, and the ether layer separated was dehydrated and concentrated to leave an oily residue. This residue was distilled under reduced pressure to give 1.9 g of p-isobutylphenylacetic acid-3-pyridylmethyl ester as a colorless liquid, boiling at 142°-145° C./1 mmHg. Analysis-Calculated for C18H21NO2 : C, 76.29; H, 7.47; N, 4.94. Found: C, 76.02; H, 7.38; N, 4.79. Mass spectrum: parent ion 283 m/e.

후처리

  1. temperaturewas heated at 65°-70° C. for 10 hours
  2. temperaturethe whole was heated at 95°-100° C. for 8 hours
  3. extractionThe resulting mixture was extracted with ether
  4. customthe ether layer separated
  5. concentrationconcentrated
  6. customto leave an oily residue
  7. distillationThis residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-de71853288824c7a8387773f47f3f4dc
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150137

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