Iodoethane → 3-butyl-1-ethyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione

HRID 2386648

반응식

HRID 2386648 반응식
[CH2:1]([N:5]1[C:13]2[N:12]=[CH:11][N:10]([CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:9]=2[C:8](=[O:21])[NH:7][C:6]1=[O:22])[CH2:2][CH2:3][CH3:4].C(=O)([O-])[O-].[K+].[K+].I[CH2:30][CH3:31]>CN(C=O)C>[CH2:1]([N:5]1[C:13]2[N:12]=[CH:11][N:10]([CH2:14][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:9]=2[C:8](=[O:21])[N:7]([CH2:30][CH3:31])[C:6]1=[O:22])[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 39938667-Benzyl-3-butylxanthine

생성물 1

HCID 592995543-butyl-1-ethyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-butyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione (0.429 g, 1.24 mmol) and potassium carbonate (0.256 g, 1.85 mmol) were suspended in DMF (8 mL), iodoethane (0.113 mL, 1.42 mmol) was added. The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was evaporated to dryness and the residue was partitioned between water and ethyl acetate. The organic layer was washed with water, followed by brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure to yield the title compound; 1H NMR (400 MHz; CDCl3) δ: 0.96 (3H, t), 1.25 (3H, t), 1.36-1.45 (2H, m), 1.72-1.76 (2H, m), 4.05-4.13 (4H, m), 5.50 (2H, s), 7.32-7.40 (5H, m), 7.52 (1H, s); m/z 327 [MH+].

후처리

  1. customThe reaction mixture was evaporated to dryness
  2. customthe residue was partitioned between water and ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2e10334914be4a08a70f1a4a74503b87
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268839B2

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