Acetic Acid → HCID 54277581、化合物

HRID 1906354

反応式

HRID 1906354 の反応式
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:12])([CH3:11])[CH:3]1[CH3:13].C(O)(=O)C.[N+:19]([O-])([OH:21])=[O:20].S(=O)(=O)(O)O>O>[N+:19]([C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[C:4]([CH3:12])([CH3:11])[CH:3]([CH3:13])[C:2]2([CH3:14])[CH3:1])([O-:21])=[O:20]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 145491,1,2,3,3-Pentamethylindan

生成物 1

HCID 54277581HCID 54277581、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

Into a 500 ml reaction vessel equipped with stirrer, thermometer, reflux condenser, addition funnel and cooling bath is placed 50 grams of 1,1,2,3,3-pentamethyl indane having the structure: ##STR36## in admixture with 100 grams of acetic acid. While maintaining the reaction mass at 25° C., 40 grams of fuming nitric acid is added over a period of 0.5 hour. The reaction mass is then stirred for a period of 6 minutes. Over a period of 10 minutes while maintaining the reaction mass at 20°-22° C., 10 grams of concentrated sulfuric acid is added to the reaction mass. The reaction mass is then heated to a temperature in the range of 26°-30° C. with stirring and maintained at that temperature for a period of four hours. At the end of the four hour period, the reaction mass is added to water and a solid is formed which precipitates out. The resulting crystals are washed with two 500 ml portions of water. The crystals melt at 99.5° C.

後処理

  1. customInto a 500 ml reaction vessel
  2. customequipped with stirrer
  3. temperaturethermometer, reflux
  4. additioncondenser, addition funnel
  5. temperaturecooling bath
  6. temperatureOver a period of 10 minutes while maintaining the reaction mass at 20°-22° C.
  7. temperatureThe reaction mass is then heated to a temperature in the range of 26°-30° C.
  8. stirringwith stirring
  9. temperaturemaintained at that temperature for a period of four hours
  10. customa solid is formed which
  11. customprecipitates out
  12. washThe resulting crystals are washed with two 500 ml portions of water
  13. custommelt at 99.5° C.

出典と根拠

ORDレコード
ord-b119787c77ef4be1ad6b4a9bd735bc73
出典データセット
uspto-grants-1987_03
特許番号
US04652400

関連ノート

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