Methyl Isocyanate → HCID 13102549, compound

HRID 1632996Notes

Reaction equation

HRID 1632996 reaction equation
[CH3:1][N:2]=[C:3]=[O:4].[O:5]([C:12]1[CH:18]=[C:17]([Cl:19])[C:16]([Cl:20])=[CH:15][C:13]=1[NH2:14])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C(N(CC)CC)C.O1CCOCC1>[O:5]([C:12]1[CH:18]=[C:17]([Cl:19])[C:16]([Cl:20])=[CH:15][C:13]=1[NH:14][C:3]([NH:2][CH3:1])=[O:4])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

Participants

5

Reactant 2

HCID 12228Methyl IsocyanateHCID 13102545HCID 13102545, compound

Product 1

HCID 13102549HCID 13102549, compound

Reagents, catalysts & solvents 2

HCID 8471TriethylamineCatalystHCID 312751,4-DioxaneSolvent

Procedure

2.0 gm (35 mmols) of methylisocyanate and two drops of triethylamine are added to a solution of 6.35 gm (25 mmols) of 2-phenoxy-4,5-dichloroaniline in 50 ml of anhydrous dioxan. The resulting solution is kept at 50°-60° C. for 15 hours. Then about 40 ml of dioxan are distilled off in vacuo and the residue is stirred with 50 ml of petrol. After cooling to 5°-10° C. for one hour, the crystalline product is suction filtered, washed with 20 ml of petrol and dried.

Workup

  1. distillationThen about 40 ml of dioxan are distilled off in vacuo
  2. temperatureAfter cooling to 5°-10° C. for one hour
  3. filtrationfiltered
  4. washwashed with 20 ml of petrol
  5. customdried

Sources & evidence

ORD record
ord-0221d4be7e164a688166ad6aa3beeb50
Source dataset
uspto-grants-1984_10
Patent number
US04478852

Reaction notes

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