Tetrahydrofuran → HCID 20256868、化合物

HRID 1763594ノート

反応式

HRID 1763594 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8](N2CCOCC2)[C:9]#N)[CH:5]=[CH:6][CH:7]=1.[O:17]1CCCC1.[OH-].[K+].[C:24](#[N:28])[C:25](C)=[CH2:26]>CO.O.C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[C:8]([CH2:9][CH:25]([CH3:26])[C:24]#[N:28])=[O:17]

参加物

8

反応物 4

HCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 31368MethacrylonitrileHCID 11241857HCID 11241857、化合物

生成物 1

HCID 20256868HCID 20256868、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 11.8 g. of α-(m-chlorophenyl)-4-morpholineacetonitrile in 50 ml. of tetrahydrofuran is added 60 drops of a 30% solution of KOH in methanol. To the solution is added 4.62 ml. of methacrylonitrile (temperature rose to 42° C.). After stirring for 1 hr., the mixture is concentrated to dryness and the residue dissolved in methylene chloride. The solution is passed through a short column of hydrous magnesium silicate and the eluent concentrated to give 15.5 g. of a yellow oil. The oil is heated (steam bath) with a mixture of 75 ml. of acetic acid and 5 ml. of water for 1 hr. and the solvent removed under vacuum. Addition of water to the residue gives 11.2 g. of crystals, m.p. 72°-75° C. Recrystallization from methylene chloride-hexane gives 8.95 g. of crystals, m.p. 79.5°-80.5° C.

後処理

  1. additionTo the solution is added 4.62 ml
  2. concentration, the mixture is concentrated to dryness
  3. dissolutionthe residue dissolved in methylene chloride
  4. concentrationthe eluent concentrated
  5. customto give 15.5 g
  6. temperatureThe oil is heated (steam bath)
  7. additionwith a mixture of 75 ml
  8. customand the solvent removed under vacuum
  9. additionAddition of water to the residue
  10. customgives 11.2 g
  11. customRecrystallization from methylene chloride-hexane
  12. customgives 8.95 g

出典と根拠

ORDレコード
ord-34588d2c589846f7a57b9da4bc0b62ab
出典データセット
uspto-grants-1978_09
特許番号
US04112095

反応ノート

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