1,1,2,2-Tetrachloroethylsulfenyl chloride → 6-propyl-1H-pyrimidin-4-one;hydrochloride
反応式
S[C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4]([CH2:9][CH2:10][CH3:11])[N:3]=1.[Cl:12]C(Cl)(SCl)C(Cl)Cl>COCCOC>[ClH:12].[OH:8][C:6]1[CH:5]=[C:4]([CH2:9][CH2:10][CH3:11])[N:3]=[CH:2][N:7]=1参加物
4
実験手順
To a slurry of 5.0 g (0.029 mol) of 2-mercapto-4-hydroxy-6-propyl pyrimidine in 50 ml of 1,2-dimethoxyethane was added 6.9 g (0.029 mol) of 1,1,2,2-tetrachloroethylsulfenyl chloride. The resulting mixture was heated at the reflux temperature for 10 minutes, and then filtered while still hot. The solvent was removed by evaporation under reduced pressure to give 8.8 g of 1,1,2,2-tetrachloroethylsulfenylmercapto)-4-hydroxy-6-propyl pyrimidine hydrochloride having a melting point of 142°-144° C. Analysis was as follows: %Cl, calc., 43.8, found 43.0; %S, calc. 15.8, found 15.5.
後処理
- temperatureThe resulting mixture was heated at the reflux temperature for 10 minutes
- filtrationfiltered while still hot
- customThe solvent was removed by evaporation under reduced pressure
出典と根拠
- ORDレコード
- ord-96dae9673bb64a038e2e1928c5909d00
- 出典データセット
- uspto-grants-1977_04
- 特許番号
- US04016275
反応ノート
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