Diethyl Ether → 2-Amino-9-(2-formyloxyethoxymethyl)adenine

HRID 2198926노트

반응식

HRID 2198926 반응식
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][O:12][CH2:13][CH2:14][OH:15])=[C:4]([NH2:16])[N:3]=1.C[CH2:18][O:19]CC>C(O)=O>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][O:12][CH2:13][CH2:14][O:15][CH:18]=[O:19])=[C:4]([NH2:16])[N:3]=1

참가 물질

4

반응물 2

HCID 3283Diethyl EtherHCID 945882,6-Diamino-9-(2-hydroxyethoxymethyl)purine

생성물 1

HCID 132555722-Amino-9-(2-formyloxyethoxymethyl)adenine

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

A solution of 2-amino-9-(2-hydroxyethoxymethyl)adenine (0.5 g) in 97% formic acid (2.5 ml) was stirred in an ice bath for 3 hours, and then at room temperature overnight. Dry ether (80 ml) was added and the mixture chilled. The solid was removed by filtration and dissolved in hot acetonitrile (125 ml); residual solids were removed by filtration. The filtrate was applied to a column containing silica gel (14 g) in acetonitrile. The column was eluted with dry acetone. The eluate was evaporated and the residual solid recrystallized from acetonitrile to give 2-amino-9-(2-formyloxyethoxymethyl)adenine (93 mg, m.p. 238°-240° C.).

후처리

  1. customat room temperature
  2. customovernight
  3. temperaturethe mixture chilled
  4. customThe solid was removed by filtration
  5. dissolutiondissolved in hot acetonitrile (125 ml)
  6. customresidual solids were removed by filtration
  7. additioncontaining silica gel (14 g) in acetonitrile
  8. washThe column was eluted with dry acetone
  9. customThe eluate was evaporated
  10. customthe residual solid recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-b56b74a977394df59ad148ac9d49b29f
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04360522

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