Chlorosulfonic acid → 4-acetamidonaphthalene-1-sulfonyl Chloride

HRID 452934

反応式

HRID 452934 の反応式
[C:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([S:15]([OH:18])(=O)=[O:16])=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[Cl:19]S(O)(=O)=O>>[C:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([S:15]([Cl:19])(=[O:18])=[O:16])=[CH:7][CH:6]=1)(=[O:3])[CH3:2]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 4169954-Acetamidonaphthalene-1-sulfonic acid

生成物 1

HCID 40255964-acetamidonaphthalene-1-sulfonyl Chloride収率 87%

実験手順

At 0° C., 4-acetamidonaphthalene-1-sulfonic acid (5 g, 19 mmol) was slowly added to chlorosulfonic acid (25 ml). The mixture was allowed to warm to RT over 30 minutes and then stirred for 2 h. After slowly adding the reaction mixture to ice water, a fine yellow precipitate formed which was filtered, washed with water and dried under vacuum to give 4-acetamidonaphthalene-1-sulfonyl chloride (4.73 g, 87%). LC/MS (10-99% CH3CN), M/Z: M+1 obs=284.0; tR=3.06 min.

後処理

  1. customa fine yellow precipitate formed which
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-fafdd180e8234385b79fd7a8a6d4ae63
出典データセット
uspto-grants-2013_07
特許番号
US08492403B2

関連ノート

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