Sodium Hydroxide → Sodium 2-(2-Propoxyethoxy)-5-nitrobenzenesulfonate

HRID 1156569

反応式

HRID 1156569 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[S:11]([O-:14])(=[O:13])=[O:12].[Na+:15].[Si]([O-])([O-])([O-])[O-].[Na+].[Na+].[Na+].[Na+].[OH-].[Na+].[CH2:27]([O:30][CH2:31][CH2:32][OH:33])[CH2:28][CH3:29]>O>[CH2:27]([O:30][CH2:31][CH2:32][O:33][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[S:11]([O-:14])(=[O:13])=[O:12])[CH2:28][CH3:29].[Na+:15]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 17756Glycol monopropyl etherHCID 26051Sodium orthosilicateHCID 70350Benzenesulfonic acid, 2-chloro-5-nitro-, sodium salt (1:1)

生成物 1

HCID 20534989Sodium 2-(2-Propoxyethoxy)-5-nitrobenzenesulfonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 26.0 g of sodium 2-chloro-5-nitrobenzenesulfonate and 5.0 g of sodium silicate (Na2O.nSiO2 ; n=about 3) was suspended in 120 ml of 2-propoxyethanol and while stirring the suspension, a solution prepared by dissolving 5.0 g of sodium hydroxide in 5 ml of water was dropwise added thereto at 65° C. over a period of 10 minutes. After the dropwise addition was completed, the resulting mixture was stirred at 65° C. for 3 hours and insoluble products were then removed by suction filtration. On allowing the filtrate to stand, solids precipitated. The solids were removed by filtration and the filtrate was condensed and dried. The addition of 100 ml of ethanol to the residue resulted in the formation of crystals. The crystals were collected by filtration, washed with isopropyl alcohol and dried at 50° C. Yield: 14.1 g.

後処理

  1. customa solution prepared
  2. additionwas dropwise added
  3. additionAfter the dropwise addition
  4. stirringthe resulting mixture was stirred at 65° C. for 3 hours
  5. custominsoluble products were then removed by suction filtration
  6. customsolids precipitated
  7. customThe solids were removed by filtration
  8. customcondensed
  9. customdried
  10. additionThe addition of 100 ml of ethanol to the residue
  11. customresulted in the formation of crystals
  12. filtrationThe crystals were collected by filtration
  13. washwashed with isopropyl alcohol
  14. customdried at 50° C

出典と根拠

ORDレコード
ord-241755ba5aa944c5896e6cf20c721636
出典データセット
uspto-grants-1982_06
特許番号
US04336322

関連ノート

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