Water → N-[4-(1,3-benzothiazol-2-yl)phenyl]benzamide

HRID 1636565

반응식

HRID 1636565 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][CH:3]=1.[C:17](Cl)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>N1C=CC=CC=1>[C:17]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][CH:7]=1)(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 7412Benzoyl chlorideHCID 2344752-(4-Aminophenyl)benzothiazole

생성물 1

HCID 720780N-[4-(1,3-benzothiazol-2-yl)phenyl]benzamide수율 82.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2-(4'-aminophenyl)benzothiazole (0.3 g, 1.32 mmol) and benzoyl chloride (0.3 ml) in pyridine (8 ml) was stirred at reflux for 2 hours, then cooled and poured into water (100 ml). The precipitate formed was filtered off, washed with water and dissolved in hot dichloromethane (12 ml). The resulting solution was cooled in an ice-bath and the solid was filtered off. The filtrate was evaporated and the residue was recrystallised from dichloromethane-methanol to give a white powder (0.36 g, 82.2%), m.p. 227.1-228.5° C.

후처리

  1. temperatureat reflux for 2 hours
  2. temperaturecooled
  3. customThe precipitate formed
  4. filtrationwas filtered off
  5. washwashed with water
  6. dissolutiondissolved in hot dichloromethane (12 ml)
  7. temperatureThe resulting solution was cooled in an ice-bath
  8. filtrationthe solid was filtered off
  9. customThe filtrate was evaporated
  10. customthe residue was recrystallised from dichloromethane-methanol

출처 및 근거

ORD 기록
ord-0af5bb72ee8c4805a786caac2d3f543a
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06034246

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