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Hydrochloric Acid → 2,6-Diethyl-2,3,6-trimethylpiperidin-4-one

HRID 66248
ノート
印刷プレビュー

反応式

HRID 66248 の反応式
[CH2:1]([C:3]1([CH3:14])N=[C:7]([CH2:9][CH3:10])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)[CH3:2].[Br-].[NH4+].Cl.C(=O)([O-])[O-:19].[K+].[K+]>CO>[CH2:1]([C:3]1([CH3:14])[CH:9]([CH3:10])[C:7](=[O:19])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 11430Potassium CarbonateHCID 25514Ammonium BromideHCID 205278902,4,6-Triethyl-2,6-dimethyl-1,2,5,6-tetrahydropyrimidine

生成物 1

HCID 221822132,6-Diethyl-2,3,6-trimethylpiperidin-4-one

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

19.6 g of 2,4,6-triethyl-2,6-dimethyl-1,2,5,6-tetrahydropyrimidine and 0.4 g of ammonium bromide were added to 200 ml of methanol. To the mixture was added dropwise 10 g of 37% hydrochloric acid at 10° C., with stirring. After completion of the addition the whole was stirred at room temperature for 4 hours and there was then added a further 20 ml of 18% hydrochloric acid. The mixture was then heated at 30°-40° C. for 7 hours and allowed to stand over night at room temperature. The mixture was made alkaline with 40% aqueous potassium carbonate solution and, after methanol has been distilled off under reduced pressure, the residue was extracted with ether. The ether solution was dried over potassium carbonate and the ether was removed. The residue was subjected to distillation under reduced pressure to yield 2,6-diethyl-2,3,6-trimethyl-4-oxopiperidine as an oil boiling at 91°-93° C./2 mm Hg.

後処理

  1. additionAfter completion of the addition the whole
  2. stirringwas stirred at room temperature for 4 hours
  3. temperatureThe mixture was then heated at 30°-40° C. for 7 hours
  4. waitto stand over night at room temperature
  5. distillationafter methanol has been distilled off under reduced pressure
  6. extractionthe residue was extracted with ether
  7. dry with materialThe ether solution was dried over potassium carbonate
  8. customthe ether was removed
  9. distillationThe residue was subjected to distillation under reduced pressure

出典と根拠

ORDレコード
ord-df2a8612cfb84b0fbe5a33693f26d1b4
出典データセット
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04131599

反応ノート

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