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

HRID 1579422
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HRID 1579422 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-79732d474edc47318f99d5d918641500
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931204

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