Sodium ethoxide → 2-Ethoxy-4-isopropylamino-thieno[3,4-d]pyrimidine

HRID 1579428노트

반응식

HRID 1579428 반응식
Cl[C:2]1[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=1.[CH3:15][CH2:16][O-:17].[Na+]>C(O)C>[CH2:16]([O:17][C:2]1[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[C:5]2[C:6](=[CH:8][S:9][CH:10]=2)[N:7]=1)[CH3:15]

참가 물질

4

반응물 2

HCID 2723922Sodium ethoxideHCID 215684292-Chloro-4-isopropylamino-thieno[3,4-d]pyrimidine

생성물 1

HCID 215684412-Ethoxy-4-isopropylamino-thieno[3,4-d]pyrimidine수율 68%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 4.5 g (0.02 mole) of 2-chloro-4-isopropylamino-thieno[3,4-d]pyrimidine and 0.02 mole sodium ethylate in 200 ml absolute ethyl alcohol is heated in an autoclave at 120°C. for 6 hours. It is then evaporated to dryness. The residue is taken up in a mixture of ether and water; the ether phase is washed with water till neutral pH, dried over Na2SO4, filtered and the solvent is driven off in vacuo. The remaining solid (4.4 g) is recrystallized from a mixture of ethyl acetate-hexane containing 30% ethyl acetate. 3.2 g (68% of theory) of 2-ethoxy-4-isopropylamino-thieno[3,4-d]pyrimidine are obtained. M.P. 155°-156°C.

후처리

  1. customIt is then evaporated to dryness
  2. additionThe residue is taken up in a mixture of ether and water
  3. washthe ether phase is washed with water till neutral pH
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customThe remaining solid (4.4 g) is recrystallized from a mixture of ethyl acetate-hexane containing 30% ethyl acetate

출처 및 근거

ORD 기록
ord-59af96d19bec4fbebc73795401d07572
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931204

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