Acetone → 1-Ethyl-4-nitrosopiperazine

HRID 2286503노트

반응식

HRID 2286503 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 125546241-Ethyl-4-nitrosopiperazine수율 103.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ca53af96c55a4b3ebfd9f2a20a29081c
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04267175

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