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Hydrochloric Acid → 4-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide

HRID 378302
ノート
印刷プレビュー

反応式

HRID 378302 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([NH:18]C(=O)C)=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH:5]=[C:4]([Br:22])[N:3]=1.Cl>[OH-].[Na+]>[NH2:18][C:15]1[CH:16]=[CH:17][C:12]([S:9]([NH:8][C:6]2[CH:7]=[C:2]([Br:1])[N:3]=[C:4]([Br:22])[CH:5]=2)(=[O:11])=[O:10])=[CH:13][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 10623382N-[4-(2,6-dibromo-pyridin-4-ylsulfamoyl)-phenyl]-acetamide

生成物 1

HCID 108113474-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide収率 86.5%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

6.2 g (0.0138 mol) of N-[4-(2,6-dibromo-pyridin-4-ylsulfamoyl)-phenyl]-acetamide were dissolved in 138 ml of 1N NaOH and boiled at reflux for 2 hours. After cooling the mixture was adjusted to pH 6 with 2N HCl and the precipitate which separated was filtered off. The material on the suction filter was washed well with water and dried. It was subsequently chromatographed on :silica gel with ethyl acetate/hexane 1:2→1:1. There were obtained 4.86 g (86%) of 4-amino-N-(2,6-dibromo-pyridin-4-yl)-benzenesulfonamide as beige crystals; m.p.: 220-222° C.

後処理

  1. temperatureat reflux for 2 hours
  2. temperatureAfter cooling the mixture
  3. customthe precipitate which separated
  4. filtrationwas filtered off
  5. filtrationThe material on the suction filter
  6. washwas washed well with water
  7. customdried
  8. customIt was subsequently chromatographed on :silica gel with ethyl acetate/hexane 1:2→1:1

出典と根拠

ORDレコード
ord-bb1472cf3e714bceb33edca525b336c2
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06030976

反応ノート

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