Ammonium Acetate → [2-(6-Chloro-pyridin-3-yl)-5-methyl-oxazol-4-yl]-acetic acid methyl ester

HRID 854580

반응식

HRID 854580 반응식
[CH3:1][O:2][C:3]([CH2:5][C:6](=O)[CH:7]([O:9][C:10](=O)[C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[N:13][CH:12]=1)[CH3:8])=[O:4].C([O-])(=O)C.[NH4+:24]>C(O)C>[CH3:1][O:2][C:3](=[O:4])[CH2:5][C:6]1[N:24]=[C:10]([C:11]2[CH:12]=[N:13][C:14]([Cl:17])=[CH:15][CH:16]=2)[O:9][C:7]=1[CH3:8]

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 86604585HCID 86604585, 화합물

생성물 1

HCID 58765666[2-(6-Chloro-pyridin-3-yl)-5-methyl-oxazol-4-yl]-acetic acid methyl ester수율 28.2%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

A mixture of 6-chloro-nicotinic acid 3-methoxycarbonyl-1-methyl-2-oxo-propyl ester (16.3 g, 57.1 mmol) and ammonium acetate (18.5 g, 240 mmol) in ethanol (150 mL) is heated at 80° C. for 2 h, concentrated. The residue is taken into acetic acid (330 mL) and heated to reflux overnight, concentrated. The residue is taken into ethyl acetate and washed with water, dried, concentrated, purified by column giving [2-(6-Chloro-pyridin-3-yl)-5-methyl-oxazol-4-yl]-acetic acid methyl ester (4.3 g).

후처리

  1. concentrationconcentrated
  2. temperatureheated
  3. temperatureto reflux overnight
  4. concentrationconcentrated
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated
  8. custompurified by column

출처 및 근거

ORD 기록
ord-5f10ed2fc9794b8e88d73155e565eba6
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07259175B2

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