Diethyl Ether → HCID 20031575, 화합물

HRID 1733700노트

반응식

HRID 1733700 반응식
[OH:1][N:2]1[C:6]2[CH:7]=[C:8]([Cl:11])[CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1.CCOCC.[C:17]1([S:23](Cl)(=[O:25])=[O:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>[OH-].[Na+]>[C:17]1([S:23]([O:1][N:2]2[C:6]3[CH:7]=[C:8]([Cl:11])[CH:9]=[CH:10][C:5]=3[N:4]=[N:3]2)(=[O:25])=[O:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 7369Benzenesulfonyl chlorideHCID 2327116-Chloro-1-hydroxy-1H-benzotriazole

생성물 1

HCID 20031575HCID 20031575, 화합물수율 73%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

In 1 N aqueous sodium hydroxide (50 ml) is dissolved 1-hydroxy-6-chloro-1,2,3-benzotriazole (4.5 g) and thereto is added ether (10 ml). To the solution is added benzenesulfonyl chloride (6.0 g) with stirring under ice-cooling and the mixture is stirred at the same temperature for 75 minutes. The reaction mixture is filtered to give crystals. The filtrate is extracted with ethyl acetate (150 ml), and the extract is distilled to remove the solvent. The resulting crystals are combined with those obtained above and recrystallized from benzene-n-hexane to give 1-benzenesulfonyloxy-6-chloro-1,2,3-benzotriazole (6.0 g), melting point: 110°-110.5° C. Infrared spectrum (Nujor): 1200, 1086 cm-1.

후처리

  1. temperaturecooling
  2. stirringthe mixture is stirred at the same temperature for 75 minutes
  3. filtrationThe reaction mixture is filtered
  4. customto give crystals
  5. extractionThe filtrate is extracted with ethyl acetate (150 ml)
  6. distillationthe extract is distilled
  7. customto remove the solvent
  8. customthose obtained above and
  9. customrecrystallized from benzene-n-hexane

출처 및 근거

ORD 기록
ord-a15e78ee9527406c9d90a9378732404a
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04242507

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