Methyl Isocyanate → HCID 14232110, compound

HRID 2248367Notes

Reaction equation

HRID 2248367 reaction equation
[N:1]1([NH:6][C:7]2[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=2)[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH3:13][N:14]=[C:15]=[O:16]>C1C=CC=CC=1>[N:10]1[CH:11]=[CH:12][C:7]([N:6]([N:1]2[CH:2]=[CH:3][CH:4]=[CH:5]2)[C:15]([NH:14][CH3:13])=[O:16])=[CH:8][CH:9]=1

Participants

4

Reactant 2

HCID 12228Methyl IsocyanateHCID 10797035HCID 10797035, compound

Product 1

HCID 14232110HCID 14232110, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Conditions

Temperature
50 °C

Procedure

A solution containing 4 g of N-(1H-pyrrol-1-yl)-4-pyridinamine 1.6 g of methyl isocyanate in 125 ml of benzene was stirred at 50° C. for two hours, and thereafter cooled and evaporated to 6 g of a solid. This material was purified by HPLC (silica gel, 50% ethyl acetate in dichloromethane) to give 5 g of a solid, mp 156°-160° C. This material was recrystallized twice from benzene to give 2.6 g of crystals, mp 162°-163° C.

Workup

  1. temperaturecooled
  2. customevaporated to 6 g of a solid
  3. customThis material was purified by HPLC (silica gel, 50% ethyl acetate in dichloromethane)

Sources & evidence

ORD record
ord-e3c948f8a1504d61bca877e109c06d6d
Source dataset
uspto-grants-1991_08
Patent number
US05039687

Reaction notes

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