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[Cl:1][C:2]1[C:7]([NH:8][CH:9]=O)=[C:6]([NH:11][O:12][CH2:13][CH2:14][CH2:15][O:16][CH2:17][P:18]([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[O:19])[N:5]=[C:4]([NH:26][CH:27]=[O:28])[N:3]=1>C(OC(OCC)OCC)(=O)C>[Cl:1][C:2]1[N:3]=[C:4]([NH:26][CH:27]=[O:28])[N:5]=[C:6]2[C:7]=1[N:8]=[CH:9][N:11]2[O:12][CH2:13][CH2:14][CH2:15][O:16][CH2:17][P:18]([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[O:19]참가 물질
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- 온도
- 25 °C
실험 절차
A solution of 4-chloro-6-[3-(diethoxyphosphorylmethoxy)propoxyamino]-2,5-diformamidopyrimidine (4.48 g, 10 mmol) in diethoxymethyl acetate (40 ml) was heated at 120° C. for 2.5 h. After removal of the solvent in vacuo. the residue was dissolved in methanol (50 ml) and 0.88 ammonia (2 ml) then stirred at 25° C. for 2 h. The reaction was then reduced in vacuo and co-evaporated twice with methanol before chromatography of the residue in chloroform/methanol (100:1) to give 6-chloro-9-[3-(diethoxyphosphorylmethoxy)propoxy]-2-formamidopurine (2.92 g, 69.2%) as a yellow oil. νmax (film) 3117,1709, 1612, 1577, 1508, 1244, 1027 cm-1 ; δH [(CD3)2SO] 1.23(6H, t, J7 Hz,(CH3CH2O)2), 1.97(2H, m, CH2CH2CH2), 3.74(2H, t, J6.1Hz, CH2OCH 2 P), 3 84(2H, d, J8.0 Hz, CH2P), 4.04(4H, m, (CH3CH2O)2), 4.48(2H, t, J6.3 Hz, CH2ON), 8.83(1H, s, H-8), 9.37(1H, br.s, CHO), 11.30(1H, br.s, D2O exchangeable, NH); Found: C, 40.05; H, 5.22; N, 16.85%; M+, 421.0921. C14H23ClN5O7P requires: C, 39.87; H, 5.02; N, 16.60%; M+, 421.0918.
후처리
- customAfter removal of the solvent in vacuo
- dissolutionthe residue was dissolved in methanol (50 ml)
출처 및 근거
- ORD 기록
- ord-62d1f18ed92f4e7598f949f69fae170f
- 출처 데이터셋
- uspto-grants-1991_10
- 특허 번호
- US05055458
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