Ethanol → HCID 20093979, compound
Reaction equation
[Cl:1][CH2:2][C:3]1[N:4]=[C:5]([NH:12][NH2:13])[C:6]2[S:11][CH:10]=[CH:9][C:7]=2[N:8]=1.[CH2:14](O)C>C([O-])([O-])OCC>[Cl:1][CH2:2][C:3]1[N:4]2[CH:14]=[N:13][N:12]=[C:5]2[C:6]2[S:11][CH:10]=[CH:9][C:7]=2[N:8]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 125 °C
Procedure
4. 15.7 g of 2-(chloromethyl)-4-hydrazinothieno[3,2-d]pyrimidine are suspended in 280ml of ethyl orthoformate. The suspension is heated (bath temp. 125° C.) while stirring and the ethanol which results is distilled off. After 3 h., the mixture is cooled to 0° C., the precipitate is filtered off and washed with ethanol. The product is dried in a vacuum. There are obtained 15.2 g of 5-(chloromethyl)thieno[2,3-e][1,2,4]triazolo[4,3-c]-pyrimidine. m.p. above 400° C. (dec.).
Workup
- distillationis distilled off
- temperaturethe mixture is cooled to 0° C.
- filtrationthe precipitate is filtered off
- washwashed with ethanol
- customThe product is dried in a vacuum
Sources & evidence
- ORD record
- ord-9fad027ca04f4e48a3bdb6c8122eedd6
- Source dataset
- uspto-grants-1995_02
- Patent number
- US05387585
Reaction notes
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