Sodium Sulfite → Sodium (4-nitrophenyl)methanesulfonate

HRID 1647776노트

반응식

HRID 1647776 반응식
[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]

참가 물질

5

반응물 2

HCID 24437Sodium SulfiteHCID 660114-Nitrobenzyl bromide

생성물 1

HCID 5314401Sodium (4-nitrophenyl)methanesulfonate수율 90%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8b39bbce930b423c8d549294b6187003
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05434154

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