Water → 3-Acetamido-6-(4-methoxyphenoxymethyl)benzoic acid

HRID 322232

反応式

HRID 322232 の反応式
[O-:1][C:2]1C=CC=CC=1.[Na+].[C:9]([NH:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[C:18](=[O:19])[O:17][CH2:16]2)(=[O:11])[CH3:10].[OH2:23].[C:24]1(C)[C:25](C)=[CH:26][CH:27]=[CH:28][CH:29]=1>>[C:9]([NH:12][C:13]1[CH:14]=[C:15]([C:20]([CH2:18][O:19][C:28]2[CH:27]=[CH:26][C:25]([O:1][CH3:2])=[CH:24][CH:29]=2)=[CH:21][CH:22]=1)[C:16]([OH:23])=[O:17])(=[O:11])[CH3:10]

参加物

5

反応物 4

HCID 962WaterHCID 7237O-XyleneHCID 5909685-Acetamido-phthalideHCID 4445035Phenolate Sodium

生成物 1

HCID 220099863-Acetamido-6-(4-methoxyphenoxymethyl)benzoic acid収率 51%

実験手順

4-Methoxyphenol (1.95 g, 15.7 mmol) was allowed to react with 28% sodium methoxide (15.7 mmol) in methanol (30 ml), at room temperature for 30 minutes. After the reaction was completed, the solvent was distilled off to obtain sodium phenoxide. The obtained sodium phenoxide and 5-acetamidophthalide obtained in Reference Example 8 (3.0 g, 15.7 mmol) were heated under reflux in xylene (30 ml) for 14 hours. The reaction mixture was poured into water and washed twice with ether (30 ml). The aqueous layer was adjusted to pH 3 with 1 mol/l hydrochloric acid and the precipitated solid was separated by filtration to give 3-acetamido-6-(4-methoxyphenoxymethyl)benzoic acid (2.49 g, 51%).

後処理

  1. temperaturewere heated
  2. washwashed twice with ether (30 ml)
  3. customthe precipitated solid was separated by filtration

出典と根拠

ORDレコード
ord-2a7813ac625d461e9b01ab2b7371fd53
出典データセット
uspto-grants-2001_04
特許番号
US06211227B1

関連ノート

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