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

HRID 322232

반응식

HRID 322232 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-2a7813ac625d461e9b01ab2b7371fd53
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211227B1

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