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Ammonia → 2,4-Diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene

HRID 839996
ノート
印刷プレビュー

反応式

HRID 839996 の反応式
[NH2:1][C:2]([CH3:10])([CH2:8][CH3:9])[CH2:3][C:4](=O)[CH2:5][CH3:6].[C:11]1(=O)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.[Br-].[NH4+:19].N.C(=O)([O-])[O-].[K+].[K+]>CO>[CH2:5]([C:4]1[CH2:3][C:2]([CH2:8][CH3:9])([CH3:10])[NH:1][C:11]2([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:19]=1)[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 222AmmoniaHCID 7967CyclohexanoneHCID 11430Potassium CarbonateHCID 25514Ammonium BromideHCID 213304575-Amino-5-methylheptan-3-one

生成物 1

HCID 213304542,4-Diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

14.3 g of the 5-amino-5-methyl-3-heptanone thus obtained were dissolved in 100 ml of methanol, and 10.0 g of cyclohexanone and 10.0 g of ammonium bromide were added to the resulting solution. Dry ammonia was then introduced into the solution at room temperature for 6 hours. The solution was then allowed to stand overnight, after which 10.0 g of potassium carbonate were added and the methanol was removed by evaporation under reduced pressure. The residue was extracted with benzene, and the benzene extract was washed with water and then dried over potassium carbonate. After removing the benzene, the residue was distilled under reduced pressure, giving 14.0 of 2,4-diethyl-4-methyl-1,5-diazaspiro[5.5]undec-1-ene (bp 93° - 94° C/1.5 mmHg).

後処理

  1. customthe methanol was removed by evaporation under reduced pressure
  2. extractionThe residue was extracted with benzene
  3. extractionthe benzene extract
  4. washwas washed with water
  5. dry with materialdried over potassium carbonate
  6. customAfter removing the benzene
  7. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-cb6c15dbdd7a4a17b5dcec5fb6bee2e8
出典データセット
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04097587

反応ノート

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