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

HRID 1579428ノート

反応式

HRID 1579428 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59af96d19bec4fbebc73795401d07572
出典データセット
uspto-grants-1976_01
特許番号
US03931204

反応ノート

読み込み中…