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Diethyl Ether → 3-(Chloroacetamido)-2-hydroxyphenyl sulfonamide

HRID 1651478
ノート
印刷プレビュー

反応式

HRID 1651478 の反応式
C([C:5]1[CH:6]=[C:7]([NH:21][C:22](=[O:25])[CH2:23][Cl:24])[C:8]([O:19]C)=[C:9]([S:11]([NH:14]C(C)(C)C)(=[O:13])=[O:12])[CH:10]=1)(C)(C)C.[Cl-].[Al+3].[Cl-].[Cl-].C1(C)C=CC=C(C)C=1.C(OCC)C>O>[Cl:24][CH2:23][C:22]([NH:21][C:7]1[C:8]([OH:19])=[C:9]([S:11]([NH2:14])(=[O:12])=[O:13])[CH:10]=[CH:5][CH:6]=1)=[O:25]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 7929M-XyleneHCID 6451240Aluminum(III) ChlorideHCID 150295875-t-butyl-2-methoxy-3-(chloroacetamido) phenyl N-t-butylsulfonamide

生成物 1

HCID 150295883-(Chloroacetamido)-2-hydroxyphenyl sulfonamide

試薬・触媒・溶媒 1

HCID 962Water
溶媒

反応条件

温度
95 °C

実験手順

A mixture of 5-t-butyl-2-methoxy-3-(chloroacetamido) phenyl-N-t-butyl-sulfonamide (8.0 g), aluminium chloride (16.4 g) and m-xylene (80 ml) was heated at 95° C. with stirring for 16 hours under nitrogen. The mixture was then poured into a beaker containing diethyl ether (300 ml) and water (300 ml) and stirred at ambient temperature for 15 minutes. The organic layer is separated and dried over sodium sulphate and concentrated under vacuum in order to remove all diethyl ether. The residual solution was cooled and hexane added to precipitate the title compound (4.7 g).

後処理

  1. additionThe mixture was then poured into a beaker
  2. stirringstirred at ambient temperature for 15 minutes
  3. customThe organic layer is separated
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated under vacuum in order
  6. customto remove all diethyl ether
  7. temperatureThe residual solution was cooled
  8. additionhexane added
  9. customto precipitate the title compound (4.7 g)

出典と根拠

ORDレコード
ord-1279d3f0b3a14fc394a6f06d92ccfada
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04929269

反応ノート

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