Thiophosgene → HCID 22155444, compound

HRID 1110359Notes

Reaction equation

HRID 1110359 reaction equation
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[C:10](Cl)([Cl:12])=[S:11]>C(Cl)Cl>[ClH:12].[CH3:9][O:8][C:5]1[CH:4]=[CH:3][C:2]([N:1]=[C:10]=[S:11])=[CH:7][N:6]=1

Participants

4

Reactant 2

HCID 10040ThiophosgeneHCID 811216-Methoxy-3-pyridinylamine

Product 1

HCID 22155444HCID 22155444, compoundYield 47.4%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

5-Amino-2-methoxypyridine (11 ml, 0.10 mol) is added dropwise at reflux, with stirring to a solution of thiophosgene (8.4 ml, 0.11 mol) in methylene chloride. Refluxing is continued for a further hour and cooled to room temperature. The resulting solid is filtered off, washed with ether to give 9.6 g of the title intermediate product.

Workup

  1. temperatureat reflux
  2. temperatureRefluxing
  3. waitis continued for a further hour
  4. filtrationThe resulting solid is filtered off
  5. washwashed with ether

Sources & evidence

ORD record
ord-ba1b56e83ffb4c84beabf843c5ceb10f
Source dataset
uspto-grants-1990_12
Patent number
US04975443

Reaction notes

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