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Ammonium Chloride → 5-(5-Isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-(4-methoxy-phenyl)-2,4-dihydro-[1,2,4]triazol-3-thione

HRID 1947185
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HRID 1947185 반응식
COC1C=CC([N:9]([C:14](=O)[C:15]2[CH:20]=[C:19]([CH:21]([CH3:23])[CH3:22])[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]=2[O:28][CH2:29][O:30][CH3:31])[NH:10][C:11]([NH2:13])=[S:12])=CC=1.[Cl-].[NH4+]>[OH-].[Na+]>[CH:21]([C:19]1[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]([O:28][CH2:29][O:30][CH3:31])=[C:15]([C:14]2[N:13]([C:15]3[CH:20]=[CH:19][C:18]([O:24][CH3:25])=[CH:17][CH:16]=3)[C:11](=[S:12])[NH:10][N:9]=2)[CH:20]=1)([CH3:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 25517Ammonium ChlorideHCID 866243104-Methoxyphenyl-1-[5-isopropyl-2,4-bis(methoxymethoxy)-benzoyl]thiosemicarbazide

생성물 1

HCID 598298385-(5-Isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-(4-methoxy-phenyl)-2,4-dihydro-[1,2,4]triazol-3-thione수율 171.4%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

4-methoxyphenyl-1-[5-isopropyl-2,4-bis(methoxymethoxy)-benzoyl]thiosemicarbazide (F53-03: 24.9 g, 53.7 mmol) and 5% aqueous sodium hydroxide (500 mL) were placed in a 1 L eggplant shaped flask and heated under reflux for 1 hour. After completing the reaction, the reaction mixture was neutralized with saturated aqueous ammonium chloride, and the solids deposited were collected by filtration, washed with distilled water and then dried under reduced pressure. The crude product thus obtained was purified by suspending in ethyl acetate/hexane and concentrating under reduced pressure to obtain the title compound (F53-04:20.5 g, 85.4%).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. customthe reaction
  4. filtrationthe solids deposited were collected by filtration
  5. washwashed with distilled water
  6. customdried under reduced pressure
  7. customThe crude product thus obtained
  8. customwas purified
  9. concentrationconcentrating under reduced pressure

출처 및 근거

ORD 기록
ord-8640c80a99af45dcaafb9806b37f2c0b
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399464B2

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