Chloroform → HCID 12953064, compound

HRID 904554Notes

Reaction equation

HRID 904554 reaction equation
[CH3:1][C:2]1[S:3][C:4]([CH3:19])=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]1[CH:12]=[C:13]([C:16]([NH2:18])=O)[CH:14]=[CH:15][C:7]1=[N:6]2.P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>N1C=CC=CC=1>[CH3:1][C:2]1[S:3][C:4]([CH3:19])=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]1[CH:12]=[C:13]([C:16]#[N:18])[CH:14]=[CH:15][C:7]1=[N:6]2

Participants

5

Reactant 3

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 12953063HCID 12953063, compound

Product 1

HCID 12953064HCID 12953064, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

1,3-Dimethyl-10-oxo-10H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxamide (Example 50), 0.6 g (0.0022 mol), in 10 ml of pyridine, 25 ml of phosphorus oxychloride and 25 ml of chloroform is refluxed on a steam bath for two hours. The solvents are evaporated in vacuo and the residue is treated with 100 ml of water. The resulting precipitate is filtered to give 0.3 g of 1,3-dimethyl-10-oxo-10H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carbonitrile with methanol (1:0.125); mp 242°-244° C. after recrystallization from methanol.

Workup

  1. customThe solvents are evaporated in vacuo
  2. additionthe residue is treated with 100 ml of water
  3. filtrationThe resulting precipitate is filtered

Sources & evidence

ORD record
ord-a76dd2646cd44cb780109de7d14442e7
Source dataset
uspto-grants-1980_10
Patent number
US04230707

Reaction notes

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