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

HRID 2459

反応式

HRID 2459 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0679f3c83e8041a093c3b3901f299d06
出典データセット
uspto-grants-1998_03
特許番号
US05728835

関連ノート

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