Diethyl Ether → HCID 20031575、化合物

HRID 1733700ノート

反応式

HRID 1733700 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 20031575HCID 20031575、化合物収率 73%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a15e78ee9527406c9d90a9378732404a
出典データセット
uspto-grants-1980_12
特許番号
US04242507

反応ノート

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