Sulfamic Acid → 5-Methoxy-2-nitrobenzoic acid

HRID 440555

反応式

HRID 440555 の反応式
S(=O)(=O)(O)N.[CH3:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([N+:16]([O-:18])=[O:17])=[C:12]([CH:15]=1)[CH:13]=[O:14].CC(C)=[O:21].O.Cl([O-])=O.[Na+]>O>[CH3:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([N+:16]([O-:18])=[O:17])=[C:12]([CH:15]=1)[C:13]([OH:21])=[O:14]

参加物

6

反応物 4

HCID 5987Sulfamic AcidHCID 2303715-Methoxy-2-nitrobenzaldehydeHCID 18366337Propan-2-one--water (1/1)HCID 23668197Sodium Chlorite

生成物 1

HCID 3392095-Methoxy-2-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sulfamic acid (15.73 g, 0.162 mol) is added to a solution of 5-methoxy-2-nitrobezaldehyde (19.6 g, 0.108 mol) in an acetone/water (1:1) mixture. Sodium chlorite (18.31 g, 80% real, 0.162 mol) is then added to the reaction mixture at a rate which maintains the reaction mixture temperature below 40° C. The resultant reaction mixture is stirred at room temperature for 24 hours and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extracts are combined, washed sequentially with 2N hydrochloric acid and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as a yellow solid.

後処理

  1. customthe reaction mixture temperature below 40° C
  2. customThe resultant reaction mixture
  3. extractionThe aqueous mixture is extracted with ethyl acetate
  4. washwashed sequentially with 2N hydrochloric acid and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fe3a904c9bd64944ba14beadcb52ad44
出典データセット
uspto-grants-1996_05
特許番号
US05519133

関連ノート

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