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Sodium Hydroxide → Sodium m-mesyloxybenzenesulfinate

HRID 851540
ノート
印刷プレビュー

反応式

HRID 851540 の反応式
S([O-])([O-])=O.[Na+:5].[Na+].[S:7]([O:11][C:12]1[CH:13]=[C:14]([S:18](Cl)(=[O:20])=[O:19])[CH:15]=[CH:16][CH:17]=1)([CH3:10])(=[O:9])=[O:8].[OH-].[Na+]>O>[S:7]([O:11][C:12]1[CH:13]=[C:14]([S:18]([O-:20])=[O:19])[CH:15]=[CH:16][CH:17]=1)([CH3:10])(=[O:9])=[O:8].[Na+:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 13518302m-Mesyloxybenzenesulfonyl chloride

生成物 1

HCID 23664830Sodium m-mesyloxybenzenesulfinate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of sodium sulfite (63 g; 0.5 mole) in water (400 ml) was added m-mesyloxybenzenesulfonyl chloride (67.7 g; 0.25 mole). The mixture was stirred vigorously, adding 50 percent sodium hydroxide solution as needed to maintain pH at 7 to 7.25, holding the temperature at 20° to 25° C. by means of a cold water bath. After 2 hours, a clear solution with a small amount of brown sludge was obtained. The mixture was filtered through Celite and the filtrate was poured into an evaporating dish and slowly allowed to evaporate. The first material to separate (32.5 g) was inorganic (by I. R. Spectrum). Further evaporation afforded three crops of crystalline material which was used without further purification.

後処理

  1. temperatureto maintain pH at 7 to 7.25
  2. customat 20° to 25° C.
  3. customa clear solution with a small amount of brown sludge was obtained
  4. filtrationThe mixture was filtered through Celite
  5. additionthe filtrate was poured into an evaporating dish
  6. customto evaporate
  7. customThe first material to separate (32.5 g)
  8. customFurther evaporation
  9. customafforded three crops of crystalline material which
  10. customwas used without further purification

出典と根拠

ORDレコード
ord-4610c700c61d4741a2ab538d49443110
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04385104

反応ノート

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