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Water → 2-Chloro-4-ethoxy-thieno[3,4-d]pyrimidine

HRID 1579422
ノート
印刷プレビュー

反応式

HRID 1579422 の反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=1.[CH3:12][CH2:13][O-:14].[Na+].O>C(O)C>[Cl:1][C:2]1[N:3]=[C:4]([O:14][CH2:13][CH3:12])[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 2723922Sodium ethoxideHCID 127128342,4-Dichlorothieno(3,4-d)pyrimidine

生成物 1

HCID 215684812-Chloro-4-ethoxy-thieno[3,4-d]pyrimidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

6.15 g (0.03 mole) of 2,4-dichloro-thieno[3,4-d]pyrimidine are suspended in 250 ml. of absolute alcohol at 0°C. Whilst agitating constantly a solution of 0.03 mole sodium ethylate in ethyl alcohol is added drop by drop. The speed of addition is regulated in such a manner that the temperature of the reaction medium is maintained at between 0° and 5°C. One obtains a clear solution in which a precipitate is gradually formed. When the addition is completed, the agitation is continued for a further 2 hours at ordinary temperature. The reaction mixture is then poured into 2 liters of iced water and the precipitate formed is filtered off, washed with water and then dried in vacuo. After recrystallization from toluene, 5.2 g of 2-chloro-4-ethoxythieno[3,4-d]pyrimidine are obtained (81% of theory). M.P. 136°-140°C.

後処理

  1. customat 0°C
  2. additionis added drop by drop
  3. additionThe speed of addition
  4. temperatureis maintained at between 0° and 5°C
  5. customOne obtains a clear solution in which a precipitate
  6. customis gradually formed
  7. additionWhen the addition
  8. customthe precipitate formed
  9. filtrationis filtered off
  10. washwashed with water
  11. customdried in vacuo
  12. customAfter recrystallization from toluene, 5.2 g of 2-chloro-4-ethoxythieno[3,4-d]pyrimidine
  13. customare obtained (81% of theory)

出典と根拠

ORDレコード
ord-79732d474edc47318f99d5d918641500
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931204

反応ノート

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