N,N-Dimethylaniline → HCID 86633293, compound

HRID 388403Notes

Reaction equation

HRID 388403 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][C:24]=1[Cl:25])[CH2:5][C:6]1[NH:7][C:8](=O)[C:9]2[C:14]([CH3:15])=[C:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[S:12][C:10]=2[N:11]=1.P(Cl)(Cl)([Cl:28])=O.CN(C)C1C=CC=CC=1>>[Cl:28][C:8]1[C:9]2[C:14]([CH3:15])=[C:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[S:12][C:10]=2[N:11]=[C:6]([CH2:5][C:4]2[CH:22]=[CH:23][C:24]([Cl:25])=[C:2]([Cl:1])[CH:3]=2)[N:7]=1

Participants

4

Reactant 3

HCID 949N,N-DimethylanilineHCID 24813Phosphorus oxychlorideHCID 69074827HCID 69074827, compound

Product 1

HCID 86633293HCID 86633293, compound

Procedure

Three (3.00) g of ethyl 2-(3,4-dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate and 37 mL of phosphorus oxychloride were mixed, and to which 1.4 mL of N,N-dimethylaniline was added, followed by stirring at 900 for 4 hours. The reaction liquid was poured on ice and stirred for 3 hours, and the precipitated crystals were recovered by filtration and washed with water. Drying the crystals under aeration, 3.05 g of the title compound was obtained.

Workup

  1. customThe reaction liquid
  2. additionwas poured on ice
  3. stirringstirred for 3 hours
  4. filtrationthe precipitated crystals were recovered by filtration
  5. washwashed with water
  6. customDrying the crystals under aeration

Sources & evidence

ORD record
ord-32de52b463e041bc8c68092a1e2ab9d1
Source dataset
uspto-grants-2013_02
Patent number
US08377944B2

Reaction notes

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