Hydrochloric Acid → HCID 12542616, 화합물

HRID 1648917노트

반응식

HRID 1648917 반응식
[CH:1]([N:3]1[CH2:8][CH2:7][C:6]([O:22][CH3:23])([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:5][CH2:4]1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>CCOCC>[CH3:1][N:3]1[CH2:4][CH2:5][C:6]([O:22][CH3:23])([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:7][CH2:8]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 12542615HCID 12542615, 화합물2회HCID 21226445Aluminium lithium hydride

생성물 1

HCID 12542616HCID 12542616, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

To a stirred mixture of 4.0 g of 1-formyl-4-methoxy-4-(α-phenyl-2-tolyl)piperidine, of Example 50 b, in 300 ml of anhydrous ether, 0.68 g of 95% lithium aluminum hydride and 100 ml of anhydrous ether is added dropwise the solution of 1-formyl-4-methoxy-4-(α-phenyl-2-tolyl)piperidine, followed by stirring 16 hours at room temperature. The resultant mixture is quenched under N2 with distilled water. The mixture is gravity filtered, the phases are separated and the aqueous phase is further extracted with ether. The combined organic phase is dried (K2CO3), filtered and evaporated to give an oil. The oil is dissolved in ether, cooled and acidified wth ethereal HCl. After 15 minutes of stirring, a crystalline precipitate is collected by suction filtration and dried in vacuo at 40° C. Recrystallization of the filter cake from absolute ethenol affords colorless crystals, mp 238°-239° C. of 1-methyl-4-methoxy-4-(α-phenyl-2-tolyl)piperidine.

후처리

  1. customThe resultant mixture is quenched under N2 with distilled water
  2. filtrationfiltered
  3. customthe phases are separated
  4. extractionthe aqueous phase is further extracted with ether
  5. dry with materialThe combined organic phase is dried (K2CO3)
  6. filtrationfiltered
  7. customevaporated
  8. customto give an oil
  9. temperaturecooled
  10. stirringAfter 15 minutes of stirring
  11. filtrationa crystalline precipitate is collected by suction filtration
  12. customdried in vacuo at 40° C
  13. customRecrystallization of the filter cake from absolute ethenol

출처 및 근거

ORD 기록
ord-8b90008e4d5b4502a3089e19438afc99
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414219

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