Triethylamine → HCID 13326913, compound

HRID 980846Notes

Reaction equation

HRID 980846 reaction equation
Cl[C:2](Cl)=[N:3][C:4](=[O:7])[O:5][CH3:6].[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][S:17]([C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([O:26][C:27]([F:32])([F:31])[CH:28]([F:30])[F:29])[CH:21]=2)(=[O:19])=[O:18])=[CH:12][C:11]=1[NH2:33].C(N(CC)CC)C>C(Cl)Cl>[F:32][C:27]([F:31])([O:26][C:22]1[CH:21]=[C:20]([S:17]([O:16][C:13]2[CH:14]=[CH:15][C:10]3[N:9]=[C:2]([NH:3][C:4]([O:5][CH3:6])=[O:7])[NH:33][C:11]=3[CH:12]=2)(=[O:18])=[O:19])[CH:25]=[CH:24][CH:23]=1)[CH:28]([F:30])[F:29]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 14255765Methyl (dichloromethylidene)carbamateHCID 20221102HCID 20221102, compound

Product 1

HCID 13326913HCID 13326913, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A solution of 15.6 g of methyl N-dichloromethylenecarbamate in 50 ml of methylene chloride is added slowly, with stirring, to a mixture of 38 g of 1,2-diamino-4-[3-(1,1,2,2-tetrafluoroethoxy)phenylsulfonyloxy]benzene (see Example 2), 20.2 g of triethylamine and 300 ml of methylene chloride at a temperature of about 20° C. The mixture is stirred for one hour and the precipitate is filtered off with suction and washed with diisopropyl ether. For purification, it is recrystallized from methanol, melting point 186° C.

Workup

  1. filtrationthe precipitate is filtered off with suction
  2. washwashed with diisopropyl ether
  3. customFor purification, it
  4. customis recrystallized from methanol, melting point 186° C.

Sources & evidence

ORD record
ord-3b29f37e67824b7fa0eb0f7ce2659d5b
Source dataset
uspto-grants-1987_01
Patent number
US04639463

Reaction notes

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