Sodium Sulfite → Sodium (4-nitrophenyl)methanesulfonate

HRID 1647776ノート

反応式

HRID 1647776 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].[S:12]([O-:15])([O-:14])=[O:13].[Na+:16].[Na+]>CO.O>[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8][S:12]([O-:15])(=[O:14])=[O:13])=[CH:6][CH:5]=1)([O-:3])=[O:2].[Na+:16]

参加物

5

反応物 2

HCID 24437Sodium SulfiteHCID 660114-Nitrobenzyl bromide

生成物 1

HCID 5314401Sodium (4-nitrophenyl)methanesulfonate収率 90%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A suspension of 100g (463 mmol, 1.0 equiv.) of 4-nitrobenzyl bromide and 64.2 g (509 mmol, 1.1 equiv.) of sodium sulfite in 500 mL of methanol and 500 mL of water was heated to reflux. The progress of the reaction was monitored by TLC. When the bromide was consumed, the reaction mixture was allowed to cool to room temperature. The product precipitated and was collected by filtration. It was thoroughly dried for sixteen hours at 65° C. at 0.05 mm Hg to give 100 g (90%) of sodium 4-nitrobenzyl sulfonate.

後処理

  1. temperaturewas heated to reflux
  2. customWhen the bromide was consumed
  3. customThe product precipitated
  4. filtrationwas collected by filtration
  5. customIt was thoroughly dried for sixteen hours at 65° C. at 0.05 mm Hg

出典と根拠

ORDレコード
ord-8b39bbce930b423c8d549294b6187003
出典データセット
uspto-grants-1995_07
特許番号
US05434154

反応ノート

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