Sodium Carbonate → Methanone, [1-(2-chloroethyl)-4-piperidinyl](4-fluorophenyl)-

HRID 2459

반응식

HRID 2459 반응식
Cl.[Cl:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][CH:8]([C:11](=[O:19])[C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:7][CH2:6]1.C(=O)([O-])[O-].[Na+].[Na+]>CCOCC>[Cl:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([C:11](=[O:19])[C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)[CH2:9][CH2:10]1

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 675753381-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride

생성물 1

HCID 10516150Methanone, [1-(2-chloroethyl)-4-piperidinyl](4-fluorophenyl)-수율 92.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride (800 mg, 2.61 mmol) was suspended in ether (20 ml). With cooling in an ice bath, saturated sodium carbonate aqueous solution (5 ml) was added dropwise to the suspension. The reaction solution was extracted with ether and washed with saturated brine, and the resulting organic layer was dried on anhydrous sodium carbonate. Thereafter, the organic layer was filtered through silica gel (5 g), the solvent was removed by evaporation and then the resulting residue was purified by subjecting it to a silica gel column chromatography (ether) to obtain 650 mg (92.3%) of the title compound in the form of light yellow solid.

후처리

  1. temperatureWith cooling in an ice bath
  2. extractionThe reaction solution was extracted with ether
  3. washwashed with saturated brine
  4. dry with materialthe resulting organic layer was dried on anhydrous sodium carbonate
  5. filtrationThereafter, the organic layer was filtered through silica gel (5 g)
  6. customthe solvent was removed by evaporation
  7. customthe resulting residue was purified

출처 및 근거

ORD 기록
ord-0679f3c83e8041a093c3b3901f299d06
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728835

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