Iodoethane → 1-Ethyl-4-nitroxypiperidine fumarate

HRID 1198143ノート

反応式

HRID 1198143 の反応式
[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]

参加物

6

反応物 4

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 5460307FumarateHCID 15068866HCID 15068866、化合物

生成物 1

HCID 867448961-Ethyl-4-nitroxypiperidine fumarate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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 organic 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.

後処理

  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 organic 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

出典と根拠

ORDレコード
ord-d36d7f5996b14bccb8ec0ade5a9153fa
出典データセット
uspto-grants-1994_01
特許番号
US05280031

反応ノート

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