Sodium Chloride → HCID 21311690、化合物

HRID 971985ノート

反応式

HRID 971985 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7](=O)[CH3:8].[CH3:10][NH:11][C:12]#[C:13][CH3:14].[Al].[Cl-].[Na+].[OH-].[Na+]>O.C(O)C>[CH3:10][N:11]([C:12]#[C:13][CH3:14])[CH:7]([CH3:8])[CH2:6][C:2]1[O:1][CH:5]=[CH:4][CH:3]=1

参加物

8

反応物 5

HCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 228583Furfuryl methyl ketoneHCID 5359268AluminumHCID 120837921-Propyn-1-amine, N-methyl-

生成物 1

HCID 21311690HCID 21311690、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

12.4 g. (0.1 mole) of 2-furyl-acetone are dissolved in 100 ml. of ethanol, whereupon 7.25 g. (0.105 moles) of methyl-propinyl amine are added. 3.5 g. of aluminium foiles are degressed with ethanol and thereafter activated with a solution of 1 g. of mercuric chloride and 15 g. of sodium chloride in 30 ml. of water. The activating solution is decanted after 6-8 minutes and the activated aluminum foils are washed with cold water and added to the alcoholic solution previously prepared under stirring. An exothermic reaction takes place and the temperature is kept at 15° to 30° C. by cooling. The reaction mixture is stirred for 24 hours, whereupon 30 ml. of 40% sodium hydroxide are added. The two phases are separated, the lower aqueous phase is extracted three-times with benzene. The benzene solutions are united with the previously separated alcoholic phase and evaporated. The residue consists of an organic oily layer and an aqueous phase which is extracted with benzene and the benzene solution is dried over potassium carbonate. The benzene is removed and the residue is distilled off in vacuo. Thus 6.7 g. of N-methyl-N-[1-methyl-2-(2-furyl)-ethyl]-propynyl amine are obtained. BP.: 113°-115° C./20 Hgmm; nD20 =1.4905.

後処理

  1. customThe activating solution is decanted after 6-8 minutes
  2. washthe activated aluminum foils are washed with cold water
  3. additionadded to the alcoholic solution
  4. custompreviously prepared
  5. customAn exothermic reaction
  6. customis kept at 15° to 30° C.
  7. temperatureby cooling
  8. stirringThe reaction mixture is stirred for 24 hours, whereupon 30 ml
  9. customThe two phases are separated
  10. extractionthe lower aqueous phase is extracted three-times with benzene
  11. customevaporated
  12. extractionan aqueous phase which is extracted with benzene
  13. dry with materialthe benzene solution is dried over potassium carbonate
  14. customThe benzene is removed
  15. distillationthe residue is distilled off in vacuo

出典と根拠

ORDレコード
ord-c5299534d93545298d7a7cde0f94ca5c
出典データセット
uspto-grants-1979_07
特許番号
US04162327

反応ノート

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