Fenpropidin → 1-[3-(4-Tert.butyl-cyclohexyl)-2-methyl-propyl]-piperidine

HRID 1733268노트

반응식

HRID 1733268 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH:12]([CH3:20])[CH2:13][N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]>C(O)(=O)C.Cl(O)(=O)(=O)=O.[Pt](=O)=O>[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([CH2:11][CH:12]([CH3:20])[CH2:13][N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]2)[CH2:7][CH2:6]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 1

HCID 91694Fenpropidin

생성물 1

HCID 203009121-[3-(4-Tert.butyl-cyclohexyl)-2-methyl-propyl]-piperidine

시약·촉매·용매 3

HCID 345198Adams' catalyst촉매HCID 176Acetic Acid용매2회HCID 24247Perchloric Acid용매

실험 절차

7 g of platinum dioxide and 7 g of active carbon are suspended in 500 ml of glacial acetic acid and pre-hydrogenated. Subsequently, a solution of 36.8 g of 1-[3-(p-tert.butyl-phenyl)-2-methyl-propyl]-piperidine in 1000 ml of glacial acetic acid and 67 ml of perchloric acid is added and the mixture is hydrogenated at 25° C. The catalyst is removed by filtration and the filtrate is treated with 110 g of potassium acetate dissolved in 100 ml of water. The precipitated potassium perchlorate is filtered, and the filtrate is evaporated on a rotary evaporator. The crystalline residue is made alkaline with 2-N sodium hydroxide, the free base is extracted with 500 ml of ether, washed neutral with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 1-[3-(4-tert.butyl-cyclohexyl)-2-methyl-propyl]-piperidine of boiling point 102° C./0.02 Torr.

후처리

  1. customis hydrogenated at 25° C
  2. customThe catalyst is removed by filtration
  3. additionthe filtrate is treated with 110 g of potassium acetate
  4. dissolutiondissolved in 100 ml of water
  5. filtrationThe precipitated potassium perchlorate is filtered
  6. customthe filtrate is evaporated on a rotary evaporator
  7. extractionthe free base is extracted with 500 ml of ether
  8. washwashed neutral with water
  9. dry with materialdried over sodium sulphate
  10. customevaporated
  11. distillationBy distillation there

출처 및 근거

ORD 기록
ord-d8b4ab6d3b9d492599c84de5956a9f2a
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04241058

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