Carbon Dioxide → HCID 9813967, compound

HRID 983908Notes

Reaction equation

HRID 983908 reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:13]2[C:9]([CH2:10][CH2:11][CH2:12]2)=[C:8](C(O)=O)[C:7]=1[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1.C(=O)=O>C(Cl)Cl>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:13]2[C:9](=[CH:8][C:7]=1[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1)[CH2:10][CH2:11][CH2:12]2

Participants

4

Reactant 2

HCID 280Carbon DioxideHCID 9879714HCID 9879714, compound

Product 1

HCID 9813967HCID 9813967, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

3-(2-Thienyl)-2-(4-pyridyl)-6,7-dihydro-5H-pyrrolizine-1-carboxylic acid (example 7, 0.2 g, 0.64 mmol) is heated under argon in a 10 ml flask by immersing in a metal bath at 250° C. Evolution of CO2 takes place immediately, and the substance melts and turns black. After cooling, the solidified, glassy melt is taken up in CH2Cl2 (10 ml) and filtered through Al2O3 (TSC, Baker). The filter cake is eluted with diethyl ether. The eluate is concentrated and crystallizes from ether/diisopropyl ether in the cold: white crystals 0.04 g.

Workup

  1. customby immersing in a metal bath at 250° C
  2. temperatureAfter cooling
  3. filtrationfiltered through Al2O3 (TSC, Baker)
  4. washThe filter cake is eluted with diethyl ether
  5. concentrationThe eluate is concentrated
  6. customcrystallizes from ether/diisopropyl ether in the cold: white crystals 0.04 g

Sources & evidence

ORD record
ord-6748bcd3334045a6a2a7a814427397fc
Source dataset
uspto-grants-2005_03
Patent number
US06867211B2

Reaction notes

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