Iodoethane → 1-Ethyl-4-nitroxypiperidine fumarate

HRID 1086490노트

반응식

HRID 1086490 반응식
[O:1]([CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)[N+:2]([O-:4])=[O:3].C(=O)([O-])[O-].[K+].[K+].[CH2:17](I)[CH3:18].[C:20]([O-:27])(=[O:26])/[CH:21]=[CH:22]/[C:23]([O-:25])=[O:24]>CC(C)=O>[C:20]([OH:27])(=[O:26])/[CH:21]=[CH:22]/[C:23]([OH:25])=[O:24].[CH2:17]([N:8]1[CH2:9][CH2:10][CH:5]([O:1][N+:2]([O-:4])=[O:3])[CH2:6][CH2:7]1)[CH3:18]

참가 물질

6

반응물 4

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 5460307FumarateHCID 15068866HCID 15068866, 화합물

생성물 1

HCID 867448961-Ethyl-4-nitroxypiperidine fumarate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

6.9 g. 4-Nitroxypiperidine are dissolved in 50 ml. acetone, mixed with 13.8 g. potassium carbonate and 6.1 ml. ethyl iodide and stirred for 18 hours at ambient temperature. After filtering with suction, the filtrate is evaporated, the residue is dissolved in ethyl acetate and extracted twice with aqueous sodium chloride solution. The orgainc phase is dried with anhydrous sodium sulphate. The crude product (8.2 g.) remaining after suction filtration and evaporation is converted into the fumarate by dissolving in ethanol and adding 2.7 g. fumaric acid. After filtering off with suction, there are obtained 2.6 g. of the fumarate of the title compound, i.e. 23% of theory; m.p. 131°-134° C.

후처리

  1. filtrationAfter filtering with suction
  2. customthe filtrate is evaporated
  3. dissolutionthe residue is dissolved in ethyl acetate
  4. extractionextracted twice with aqueous sodium chloride solution
  5. dry with materialThe orgainc phase is dried with anhydrous sodium sulphate
  6. filtrationafter suction filtration and evaporation
  7. dissolutionby dissolving in ethanol
  8. additionadding 2.7 g
  9. filtrationAfter filtering off with suction, there
  10. customare obtained 2.6 g

출처 및 근거

ORD 기록
ord-b2dab2d39ef8479eacbbd4585a6d4e18
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05030641

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