Water → HCID 135703167, 화합물

HRID 27580노트

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HRID 27580 반응식
[OH:1][CH:2]([CH3:14])[CH2:3][N:4]1[CH:12]=[N:11][C:10]2[C:5]1=[N:6][CH:7]=[N:8][C:9]=2N.N([O-])=[O:16].[Na+].O>C(O)(=O)C>[OH:1][CH:2]([CH3:14])[CH2:3][N:4]1[CH:12]=[N:11][C:10]2[C:9](=[O:16])[NH:8][CH:7]=[N:6][C:5]1=2

참가 물질

5

실험 절차

9-(2-Hydroxy-1-propyl)adenine (I, 4.0 g, 20.7 mmol) was suspened in 50% acetic acid (20 ml) and sodium nitrite (4 g, 58 mmol), was slowly added. The mixture was stirred at 25° for 3 hr. The resulting solution was evaporated to dryness and isopropanol added; this operation was repeated once. The solid residue was boiled in isopropanol and filtered. The filtrate was evaporated and crystallized by addition of acetone. Recrystallization was made from iso-propanol/methanol (98:2); a colorless crystalline product was obtained. Yield 3.3 g (82%); M.P. 244°-250°; uv (H2O; pH 5.5), λmax 250 nm.

후처리

  1. customThe resulting solution was evaporated to dryness and isopropanol
  2. additionadded
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customcrystallized by addition of acetone
  6. customRecrystallization
  7. customa colorless crystalline product was obtained

출처 및 근거

ORD 기록
ord-9e325db5ddec4fedac15f39e5a1f0158
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221910

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