p-Toluenesulfonic acid monohydrate → Methyl 2-acetamino-4-[(2-{1-[5-(4-t-butylphenyl)-4-hydroxy-3-thienyl]ethylidene}hydrazino)carbonyl]benzoate

HRID 1881615노트

반응식

HRID 1881615 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[S:12][CH:13]=[C:14]([C:17]([CH3:19])=O)[C:15]=2[OH:16])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[NH:20]([C:24]1[CH:33]=[C:32]([C:34]([NH:36][NH2:37])=[O:35])[CH:31]=[CH:30][C:25]=1[C:26]([O:28][CH3:29])=[O:27])[C:21]([CH3:23])=[O:22].O.S(C1C=CC(C)=CC=1)(O)(=O)=O>C(O)(C)C>[NH:20]([C:24]1[CH:33]=[C:32]([C:34]([NH:36][N:37]=[C:17]([C:14]2[C:15]([OH:16])=[C:11]([C:8]3[CH:9]=[CH:10][C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:6][CH:7]=3)[S:12][CH:13]=2)[CH3:19])=[O:35])[CH:31]=[CH:30][C:25]=1[C:26]([O:28][CH3:29])=[O:27])[C:21]([CH3:23])=[O:22]

참가 물질

5

반응물 3

HCID 521998p-Toluenesulfonic acid monohydrateHCID 442072892-(4-t-Butylphenyl)-3-hydroxy-4-methylcarbonylthiopheneHCID 67050072Methyl 2-acetamino-4-hydrazinocarbonylbenzoate

생성물 1

HCID 86604757Methyl 2-acetamino-4-[(2-{1-[5-(4-t-butylphenyl)-4-hydroxy-3-thienyl]ethylidene}hydrazino)carbonyl]benzoate수율 83%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a suspension of 2-(4-t-butylphenyl)-3-hydroxy-4-methylcarbonylthiophene (54.8 mg, 0.2 mmol) and methyl 2-acetamino-4-hydrazinocarbonylbenzoate (50.2 mg, 0.2 mmol) in isopropyl alcohol (2 mL), tosylic acid monohydrate (11.4 mg, 0.06 mmol) was added, and the mixture was heated with reflux for 12 hours. The precipitated solid was filtered to obtain 84 mg of the desired product as a pale yellow solid (yield 83%).

후처리

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperaturewith reflux for 12 hours
  4. filtrationThe precipitated solid was filtered

출처 및 근거

ORD 기록
ord-82ff34358ab34df0af20f559c01af6dc
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318796B2

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