Sodium Hydroxide → HCID 2645656、化合物

HRID 1291701ノート

反応式

HRID 1291701 の反応式
S([O-])([O-])=O.[Na+].[Na+].[C:7]([C:10]1[CH:11]=[CH:12][C:13]([Cl:20])=[C:14]([S:16](Cl)(=[O:18])=[O:17])[CH:15]=1)([OH:9])=[O:8].[OH-].[Na+]>O>[Cl:20][C:13]1[CH:12]=[CH:11][C:10]([C:7]([OH:9])=[O:8])=[CH:15][C:14]=1[S:16]([OH:18])=[O:17]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 756134-Chloro-3-(chlorosulphonyl)benzoic acid

生成物 1

HCID 2645656HCID 2645656、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

157.55 g of sodium sulfite (1.25 mol) were dissolved in 725 ml of water and heated to 70° C. At this temperature, 255.08 g of 5-carboxy-2-chlorobenzenesulfonyl chloride were added in portions, the pH (electrode) being kept between 8 and 10 by continuous addition of 320 ml of half-concentrated sodium hydroxide solution (the reaction is slightly exothermic). After the end of the addition, the mixture was subsequently stirred at 70° C. for 2 hours. As soon as the reaction had ended, 5 g of active carbon were added, and after 30 minutes the mixture was filtered hot through a clarifying layer and diluted with 600 ml of water. The solution was allowed to cool to 15°-20° C. and was adjusted to pH 0 using 250 ml of conc. hydrochloric acid, the viscous suspension was stirred in an ice bath for a further 30 minutes and the mixture was then stood well closed in a refrigerator over the weekend. The precipitate was filtered off with suction, washed once with 100 ml of 2N hydrochloric acid and then sucked dry in a stream of air. The substance was sucked dry in vacuo at 50° C.

後処理

  1. additionAfter the end of the addition
  2. addition5 g of active carbon were added
  3. filtrationafter 30 minutes the mixture was filtered hot through a clarifying layer
  4. additiondiluted with 600 ml of water
  5. temperatureto cool to 15°-20° C.
  6. stirringthe viscous suspension was stirred in an ice bath for a further 30 minutes
  7. customthe mixture was then stood well closed in a refrigerator over the weekend
  8. filtrationThe precipitate was filtered off with suction
  9. washwashed once with 100 ml of 2N hydrochloric acid
  10. customsucked dry in a stream of air
  11. customThe substance was sucked dry in vacuo at 50° C.

出典と根拠

ORDレコード
ord-ea698398e4594060b8ae8c75d89cab50
出典データセット
uspto-grants-1998_05
特許番号
US05753710

反応ノート

読み込み中…