Sulfuric Acid → Cyclohexanone Oxime

HRID 234110

反応式

HRID 234110 の反応式
S(=O)(=O)(O)[OH:2].[CH2:6]([OH:11])[CH2:7][CH2:8][CH2:9][CH3:10].[C:12]1(=[N:18][OH:19])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+]>[C:12]1(=[N:18][OH:19])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.[C:6]1(=[O:11])[CH2:12][CH2:10][CH2:9][CH2:8][CH2:7]1.[C:12]1(=[O:2])[NH:18][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]1

参加物

7

反応物 3

HCID 1118Sulfuric AcidHCID 62761-PentanolHCID 7517Cyclohexanone Oxime

生成物 3

HCID 7517Cyclohexanone OximeHCID 7768CaprolactamHCID 7967Cyclohexanone

試薬・触媒・溶媒 1

HCID 3423265Sodium Lauryl Sulfate溶媒

反応条件

温度
25 °C

実験手順

Take 200 ml of aqueous solution of 3.0N sulfuric acid in a round bottom flask. Dissolve in this solution 16 grams of sodium dodecyl sulfate (SDS) and 5.3 gm 1-pentanol by mild stirring. A microemulsion is thus formed. Keep the flask in a water bath maintained at temperature of 25° C. To this microemulsion, add 10.0 gm of cyclohexanone oxime and stir the mixture mildly for 2 hours. Remove the flask from the water bath and neutralize the solution using aqueous solution of ammonia. Filter the solution using Whatman No. 1 filter paper. Measure the amount of filtrate and the residue and extract the filtrate with 100 ml of benzene in steps of 50, 25, and 25 ml respectively. Analyze the benzene layer, the aqueous layer and the residue obtained as above by Gas Chromatography for the amount of cyclohexanone oxime, cyclohexanone and caprolactam.

後処理

  1. customA microemulsion is thus formed
  2. customRemove the flask from the water bath
  3. filtrationFilter the solution
  4. filtration1 filter paper
  5. extractionMeasure the amount of filtrate and the residue and extract the filtrate with 100 ml of benzene in steps of 50, 25, and 25 ml respectively

出典と根拠

ORDレコード
ord-5e46c52f020e44479e549eb560fcecaf
出典データセット
uspto-grants-1997_01
特許番号
US05594137

関連ノート

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