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Hydrochloric Acid → 8-Benzyl-3,8-diazabicyclo[3.2.1]octane

HRID 1743696
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HRID 1743696 반응식
[CH2:1]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][N:11](CC=C)[CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN1C(=O)CC(=O)N(C)C1=O.P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.Cl>C(Cl)Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH2:1]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][NH:11][CH2:12]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 69860Dimethylbarbituric acidHCID 222355893-Allyl-8-benzyl-3,8-diazabicyclo[3.2.1]octane

생성물 1

HCID 120798988-Benzyl-3,8-diazabicyclo[3.2.1]octane

시약·촉매·용매 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 6344Dichloromethane용매

실험 절차

A mixture of 8-benzyl-3-(2-propenyl)-3,8-diazabicyclo[3.2.1]octane (22.2 g, 92.7 mmol), 1,3-dimethylbarbituric acid (21.5 g, 137.0 mmol), Pd2(dba)3 (5 g, 5 mmol) and P(C6H5)3 (5.2 g, 20.0 mmol) in methylene chloride (500 mL) was heated at reflux for 16 h. The reaction was poured into 1 N HCl (250 mL) at 0° C. The aqueous acidic layer was separated and made basic with 6 N NaOH, then extracted with ethyl acetate (2×150 mL).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. customThe aqueous acidic layer was separated
  4. extractionextracted with ethyl acetate (2×150 mL)

출처 및 근거

ORD 기록
ord-6033c950d8224b7e93c47b8d72d7f65b
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07012074B2

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