Ammonia → 6-chloro-3-oxo-2,3-dihydro-1H-indene-5-sulfonamide

HRID 65932ノート

反応式

HRID 65932 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[S:11](Cl)(=[O:13])=[O:12])[C:7](=[O:15])[CH2:6][CH2:5]2.[NH3:16]>>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[S:11](=[O:13])(=[O:12])[NH2:16])[C:7](=[O:15])[CH2:6][CH2:5]2

参加物

3

反応物 2

HCID 222AmmoniaHCID 221190346-chloro-3-oxo-2,3-dihydro-1H-indene-5-sulfonyl chloride

生成物 1

HCID 227563846-chloro-3-oxo-2,3-dihydro-1H-indene-5-sulfonamide

実験手順

99.6 Grams of 5-chloro-6-chlorosulfonyl-1-indanone are introduced portionwise into 700 ml of liquid ammonia. The solvent is allowed to evaporate and the residue is dissolved in water, is heated within a short time on the water-bath and is filtered after the addition of active charcoal. The solution is acidified with hydrochloric acid to a pH of 2, the precipitate is filtered off with suction and is washed with water. The melting point of 5-chloro-6-sulfamoyl-1-indanone is in the range of from 205° to 208° C., and after recrystallization from a mixture of acetone and water it is 216° to 218° C.

後処理

  1. customto evaporate
  2. dissolutionthe residue is dissolved in water
  3. temperatureis heated within a short time on the water-bath
  4. filtrationis filtered
  5. additionafter the addition of active charcoal
  6. filtrationthe precipitate is filtered off with suction
  7. washis washed with water
  8. customis in the range of from 205° to 208° C.
  9. customafter recrystallization
  10. additionfrom a mixture of acetone and water it
  11. customis 216° to 218° C.

出典と根拠

ORDレコード
ord-2122063c84c848c19820fb2b2aa12265
出典データセット
uspto-grants-1978_12
特許番号
US04129656

反応ノート

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