Water → HCID 20300028、化合物

HRID 1733698ノート

反応式

HRID 1733698 の反応式
[OH:1][N:2]1[C:6]2[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1.[C:14]1([S:20](Cl)(=[O:22])=[O:21])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.O.C(OCC)(=O)C>[OH-].[Na+]>[C:14]1([S:20]([O:1][N:2]2[C:6]3[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=3[N:4]=[N:3]2)(=[O:22])=[O:21])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 7369Benzenesulfonyl chlorideHCID 8857Ethyl AcetateHCID 1528171-Hydroxy-6-nitrobenzotriazole

生成物 1

HCID 20300028HCID 20300028、化合物収率 53.6%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

In 1 N aqueous sodium hydroxide (45 ml) is dissolved 1-hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g). To the solution is added dropwise benzenesulfonyl chloride (7.0 g) with stirring at room temperature and further are added thereto water (50 ml) and ethyl acetate (100 ml) and the mixture is stirred for 1 hour. The ethyl acetate layer is separated, dried over magnesium sulfate-charcoal, filtered and concentrated until it becomes about 30 ml. n-Hexane (50 ml) is thereto added and the mixture is allowed to stand. The precipitated crystals are separated by filtration and dried to give faint yellow prisms of 1-benzenesulfonyloxy-6-nitro-1,2,3-benzotriazole (6.8 g), melting point: 122°-124° C. The product is recrystallized from ethyl acetate-n-hexane to give a pure product: melting point: 124° C.

後処理

  1. additionfurther are added
  2. customThe ethyl acetate layer is separated
  3. dry with materialdried over magnesium sulfate-charcoal
  4. filtrationfiltered
  5. concentrationconcentrated until it
  6. additionn-Hexane (50 ml) is thereto added
  7. customThe precipitated crystals are separated by filtration
  8. customdried

出典と根拠

ORDレコード
ord-e99f9d1d4a5d4ee4bb83db65fa9f4ce8
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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