Diethyl Sulfate → HCID 178467038、化合物

HRID 442489ノート

反応式

HRID 442489 の反応式
[CH3:1][S:2][C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5]([OH:10])[N:4]=1.S(OCC)(O[CH2:15][CH3:16])(=O)=O.S([O-])([O-])(=O)=O.[Na+].[Na+]>[OH-].[Na+]>[CH3:1][S:2][C:3]1[N:8]=[C:7]([O:9][CH2:15][CH3:16])[CH:6]=[C:5]([OH:10])[N:4]=1

参加物

5

反応物 3

HCID 6163Diethyl SulfateHCID 24436Sodium SulfateHCID 178503559HCID 178503559、化合物

生成物 1

HCID 178467038HCID 178467038、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

31.6 g (0.2 mol) of 2-methylthio-4,6-dihydroxypyrimidine are added, while stirring well, to 100 cc of sodium hydroxide solution 2N and the mixture is stirred at 50° for half an hour. 34.0 g (0.22 mol) of diethyl sulphate are then added dropwise and with stirring, at 50°; by the addition of sodium sulphate 2N the pH value is kept at between 8 and 8.2. Towards the end of the dropwise addition a precipitate is obtained. The mixture is subsequently stirred at 50° for 1 further hour, cooled to 0° and filtered. The precipitate is washed with cold ethanol, then with ether and dried in a high vacuum at 80°. The obtained white powder has a M.P. of 185°-187°.

後処理

  1. stirringwith stirring, at 50°
  2. additionTowards the end of the dropwise addition a precipitate
  3. customis obtained
  4. stirringThe mixture is subsequently stirred at 50° for 1 further hour
  5. temperaturecooled to 0°
  6. filtrationfiltered
  7. washThe precipitate is washed with cold ethanol
  8. dry with materialwith ether and dried in a high vacuum at 80°

出典と根拠

ORDレコード
ord-413dbafac13b4f5692a3dfa5e83964ca
出典データセット
uspto-grants-1977_08
特許番号
US04045561

反応ノート

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