Methyl Isocyanate → HCID 21431632, compound

HRID 2397656Notes

Reaction equation

HRID 2397656 reaction equation
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[NH:20][N:19]=[CH:18][C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1.[CH3:23][N:24]=[C:25]=[O:26]>O1CCCC1>[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[C:7](=[CH:18][N:19]([C:25](=[O:26])[NH:24][CH3:23])[N:20]=3)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 12228Methyl IsocyanateHCID 21431654HCID 21431654, compound

Product 1

HCID 21431632HCID 21431632, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

The solution of 1.45 g of 8-chloro-6-(2-fluorophenyl)-1H,4H-pyrazolo[4,3-d](2)benzazepine and 1.4 ml of methylisocyanate in 20 ml of tetrahydrofuran is refluxed for 5 hours under nitrogen and evaporated under reduced pressure. The residue is taken up in chloroform, the solution filtered through a column of 15 g of silica gel, the first fractions collected, evaporated and the residue recrystallized from diethyl ether, to yield the 8-chloro-6-(2-fluorophenyl)-2-methylcarbamoyl-2H,4H-pyrazolo[4,3-d](2)benzazepine melting at 192°-193°.

Workup

  1. customevaporated under reduced pressure
  2. filtrationthe solution filtered through a column of 15 g of silica gel
  3. customthe first fractions collected
  4. customevaporated
  5. customthe residue recrystallized from diethyl ether

Sources & evidence

ORD record
ord-4e0cf6526ad44dcf83ce760d750947bb
Source dataset
uspto-grants-1977_05
Patent number
US04022801

Reaction notes

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