Chloroform → HCID 12862372, compound

HRID 1155871Notes

Reaction equation

HRID 1155871 reaction equation
[CH3:1][CH:2]([C:4]1[S:20][C:7]2[N:8]=[C:9]3[CH:16]=[CH:15][C:14]([C:17]([NH2:19])=O)=[CH:13][N:10]3[C:11](=[O:12])[C:6]=2[CH:5]=1)[CH3:3].C(Cl)(Cl)Cl>P(Cl)(Cl)(Cl)=O>[CH3:3][CH:2]([C:4]1[S:20][C:7]2[N:8]=[C:9]3[CH:16]=[CH:15][C:14]([C:17]#[N:19])=[CH:13][N:10]3[C:11](=[O:12])[C:6]=2[CH:5]=1)[CH3:1]

Participants

4

Reactant 2

HCID 6212ChloroformHCID 12862365HCID 12862365, compound

Product 1

HCID 12862372HCID 12862372, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

2-(1-Methylethyl)-4-oxo-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7-carboxamide (Example 15), 8.7 g (0.0303 mol), in 250 ml of phosphorus oxychloride and 250 ml of chloroform is refluxed on a steam bath for four hours under nitrogen. The chloroform and excess phosphorus oxychloride are evaporated in vacuo and the residue is treated with 2 L of ice water. The resulting precipitate is filtered to give 5.3 g of 2-(1-methylethyl)-4-oxo-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7-carbonitrile; mp 225°-226° C. after recrystallization from pyridine.

Workup

  1. customThe chloroform and excess phosphorus oxychloride are evaporated in vacuo
  2. additionthe residue is treated with 2 L of ice water
  3. filtrationThe resulting precipitate is filtered

Sources & evidence

ORD record
ord-d572b8da5fc54628aab77268a26dd5a0
Source dataset
uspto-grants-1982_06
Patent number
US04332947

Reaction notes

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