Acetone → 1-Ethyl-4-nitrosopiperazine

HRID 2286503ノート

反応式

HRID 2286503 の反応式
[CH2:1](I)[CH3:2].CC(C)=O.[N:8]([N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[O:9].C(=O)([O-])[O-].[K+].[K+]>O>[CH2:14]([N:13]1[CH2:2][CH2:1][N:10]([N:8]=[O:9])[CH2:11][CH2:12]1)[CH3:15]

参加物

6

反応物 4

HCID 180AcetoneHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 21845N-Nitrosopiperazine

生成物 1

HCID 125546241-Ethyl-4-nitrosopiperazine収率 103.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Ethyl iodide (8.13 g, 0.052 mole) was added to acetone (80 ml) containing N-nitroso piperazine (6.0 g, 0.052 mole) (prepared as described in U.S. Pat. No. 2,907,767) and anhydrous potassium carbonate (7.3 g, 0.052 mole). The mixture was heated under reflux for 24 hours, cooled, treated with water (50 ml) evaporated to 1/2 volume and extracted with ether (3×150 ml). The combined extracts were dried (K2CO3) filtered and evaporated in vacuo to yield N-ethyl-N'-nitrosopiperazine (7.71 g, 98%), as a straw coloured oil.

後処理

  1. customprepared
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 24 hours
  4. temperaturecooled
  5. customevaporated to 1/2 volume
  6. extractionextracted with ether (3×150 ml)
  7. dry with materialThe combined extracts were dried (K2CO3)
  8. filtrationfiltered
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-ca53af96c55a4b3ebfd9f2a20a29081c
出典データセット
uspto-grants-1981_05
特許番号
US04267175

反応ノート

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