Dimethyl Sulfate → (Methoxymethyl)cyclododecane

HRID 2198797ノート

反応式

HRID 2198797 の反応式
[NH2-].[Na+].[OH:3][CH2:4][CH:5]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.S(OC)(O[CH3:21])(=O)=O.[OH-].[Na+]>C1(C)C(C)=CC=CC=1>[CH:5]1([CH2:4][O:3][CH3:21])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1

参加物

6

反応物 4

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 24533Sodium amideHCID 74686Cyclododecanemethanol

生成物 1

HCID 3018712(Methoxymethyl)cyclododecane

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

25 g (0.65 mol) of sodium amide was introduced into 150 ml of xylene and heated to boiling under agitation. Within one hour, 99 g (0.5 mol) of hydroxymethylcyclododecane, dissolved in 750 ml of xylene, was added dropwise to the boiling suspension. To complete the alcoholate formation the mixture was heated for another two hours under reflux. Thereafter 44 g (0.35 mol) of dimethyl sulfate was added dropwise. The reaction mixture was heated under reflux for another four hours and then poured into a mixture of ice and 35 g of sodium hydroxide. The organic phase was washed with water, dried with Na2SO4, and then distilled.

後処理

  1. temperatureheated
  2. additionwas added dropwise to the boiling suspension
  3. temperaturewas heated for another two hours
  4. temperatureunder reflux
  5. temperatureThe reaction mixture was heated
  6. temperatureunder reflux for another four hours
  7. washThe organic phase was washed with water
  8. dry with materialdried with Na2SO4
  9. distillationdistilled

出典と根拠

ORDレコード
ord-cb053392c31642de9e05f9ccbe32356c
出典データセット
uspto-grants-1982_11
特許番号
US04359588

反応ノート

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