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

HRID 854580

反応式

HRID 854580 の反応式
[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]

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 86604585HCID 86604585、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-5f10ed2fc9794b8e88d73155e565eba6
出典データセット
uspto-grants-2007_08
特許番号
US07259175B2

関連ノート

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