Methyl Isocyanate → HCID 15622814, compound

HRID 1199959Notes

Reaction equation

HRID 1199959 reaction equation
[O:1]=[C:2]1[CH2:6][CH2:5][CH2:4][N:3]1[CH2:7][C:8]([N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[O:9].[CH3:16][N:17]=[C:18]=[O:19]>C(Cl)Cl>[CH3:16][NH:17][C:18]([N:13]1[CH2:12][CH2:11][N:10]([C:8](=[O:9])[CH2:7][N:3]2[CH2:4][CH2:5][CH2:6][C:2]2=[O:1])[CH2:15][CH2:14]1)=[O:19]

Participants

4

Reactant 2

HCID 12228Methyl IsocyanateHCID 7107340HCID 7107340, compound

Product 1

HCID 15622814HCID 15622814, compoundYield 96.4%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

700 mg (3.31 mmol) of (2-oxopyrrolidin-1-yl)acetylpiperazine was dissolved in 10.5 ml of CH2Cl2, and 0.215 ml (3.64 mmol) of methyl isocyanate was added to the mixture under ice-cooling, and the mixture was warmed to room temperature and stirred for 1 hr. After evaporating CH2Cl2, the precipitated crystals were washed with Et2O and collected by filtration. By recrystallizing from EtOH-Et2O, 856 mg of the objective compound (yield: 96.3%) was obtained as colorless prisms.

Workup

  1. temperaturecooling
  2. customAfter evaporating CH2Cl2
  3. washthe precipitated crystals were washed with Et2O
  4. filtrationcollected by filtration
  5. customBy recrystallizing from EtOH-Et2O

Sources & evidence

ORD record
ord-08a840188d554835bca8f60aeda5f042
Source dataset
uspto-grants-1990_02
Patent number
US04904663

Reaction notes

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