Chloroform → HCID 13105814, compound

HRID 1758770Notes

Reaction equation

HRID 1758770 reaction equation
[O:1]=[C:2]1[N:6]2[C:7]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:8]=3[CH:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[O:10][CH2:11][C:5]2=[N:4][N:3]1[CH3:24].C(Cl)(Cl)Cl.C(Cl)(=O)OCC>C(N(CC)CC)C>[O:1]=[C:2]1[N:6]2[C:7]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:8]=3[CH:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[O:10][CH2:11][C:5]2=[N:4][N:3]1[CH2:24][CH2:5][N:6]([CH3:7])[CH3:2]

Participants

5

Reactant 3

HCID 6212ChloroformHCID 10928Ethyl chloroformateHCID 13068324HCID 13068324, compound

Product 1

HCID 13105814HCID 13105814, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

Compound 33 is mixed with chloroform (20 ml), triethylamine (0.708 g), and ethyl chlorocarbonate (0.76 g), and the mixture is stirred at room temperature for 20 minutes, then refluxed under heating for 3.5 hours, and washed with water. The chloroform layer is dried and concentrated to give crystalline Compound 34 (2.15 g), which is recrystallized from ethanol.

Workup

  1. temperaturerefluxed
  2. temperatureunder heating for 3.5 hours
  3. washwashed with water
  4. dry with materialThe chloroform layer is dried
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-52d2ea996199460ba21f7266123274f9
Source dataset
uspto-grants-1983_02
Patent number
US04374842

Reaction notes

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