Hydrochloric Acid → 4-(Diphenylmethyl)piperidine hydrochloride

HRID 2297513노트

반응식

HRID 2297513 반응식
[ClH:1].[C:2]1([C:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[C:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[H][H]>[C].[Pd].CO>[ClH:1].[C:2]1([CH:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]2)[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 135045484-Diphenylmethylenepiperidine hydrochlorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 230040934-(Diphenylmethyl)piperidine hydrochloride수율 38.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

4-diphenylmethylenepiperidine hydrochloride (6.21 g) was added to methanol (30 ml) and the atmosphere was replaced with argon. To the mixture, 10% palladium-carbon (1.54 g) and a small amount,of concentrated hydrochloric acid were added and the atmosphere was replaced with hydrogen, followed by allowing the mixture to react at 3.5 atm at room temperature for 10.5 hours. Then 10% palladium-carbon was removed through Celite and the filtrate was concentrated. The residue was again dissolved in methanol (30 ml) and 10% palladium-carbon (10 g) and a small amount of hydrochloric acid were added. The atmosphere was replaced with hydrogen, and the mixture was allowed to react at 3.5 atm at room temperature for 21 hours. The reaction mixture was filtered through Celite and the filtrate was concentrated, followed by recrystallizing the residue from methanol/ether to obtain 2.38g of 4-diphenylmethylpiperidine hydrochloride. Yield: 38%.

후처리

  1. customto react at 3.5 atm at room temperature for 10.5 hours
  2. customThen 10% palladium-carbon was removed through Celite
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was again dissolved in methanol (30 ml)
  5. addition10% palladium-carbon (10 g) and a small amount of hydrochloric acid were added
  6. customto react at 3.5 atm at room temperature for 21 hours
  7. filtrationThe reaction mixture was filtered through Celite
  8. concentrationthe filtrate was concentrated
  9. customby recrystallizing the residue from methanol/ether

출처 및 근거

ORD 기록
ord-26dd78430b7e40fcbf63646fbe236b18
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06492364B1

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