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1-Bromo-3-chloropropane → 2-(3-Chloropropyl)octahydrocyclopenta[c]pyrrole

HRID 712434
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HRID 712434 반응식
Cl.[CH2:2]1[CH:6]2[CH2:7][CH2:8][CH2:9][CH:5]2[CH2:4][NH:3]1.C([O-])([O-])=O.[K+].[K+].[Cl:16][CH2:17][CH2:18][CH2:19]Br>CC(C)=O>[Cl:16][CH2:17][CH2:18][CH2:19][N:3]1[CH2:4][CH:5]2[CH2:9][CH2:8][CH2:7][CH:6]2[CH2:2]1
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참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 21572123Cyclopenta(c)pyrrole, octahydro-, hydrochloride (1:1)

생성물 1

HCID 867294842-(3-Chloropropyl)octahydrocyclopenta[c]pyrrole수율 56.63%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a suspension of octahydrocyclopenta[c]pyrrole hydrochloride (5.00 g, 33.86 mmol) in acetone (150 mL) was added K2CO3 (35.68 g, 101.59 mmol) and 1-chloro-3-bromopropane (10.56 g, 67.72 mmol) in turn. The reaction mixture was heated to reflux for 12 h under N2. The solvent was removed, and the residue was treated with 200 mL of EtOAc. The mixture was washed with water followed by brine. The mixture was dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was chromatographed with a silica gel column (eluting agent: 1:1 (v/v) PE/EtOAc) to afford the title compound (3.06 g, 56.63%). The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 188.7 (M+1); 1H NMR (400 MHz, CDCl3) δ: 1.24-1.28 (m, 1H), 1.38-1.40 (m, 2H), 2.06 (m, 1H), 2.46-2.50 (m, 2H), 2.56-2.57 (m, 3H), 2.63-2.68 (m, 2H), 2.70 (d, J=2.24 Hz, 2H), 2.71-2.73 (m, 2H), 3.60 (m, 2H) ppm.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 12 h under N2
  3. customThe solvent was removed
  4. additionthe residue was treated with 200 mL of EtOAc
  5. washThe mixture was washed with water
  6. dry with materialThe mixture was dried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was chromatographed with a silica gel column (eluting agent: 1:1 (v/v) PE/EtOAc)

출처 및 근거

ORD 기록
ord-dd7d1d83674549b4a29bbff04c4ce034
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181277B2

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