Water → HCID 135703167、化合物

HRID 27580ノート

反応式

HRID 27580 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 19429-(2-Hydroxypropyl)adenineHCID 23668193Sodium Nitrite

生成物 1

HCID 135703167HCID 135703167、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e325db5ddec4fedac15f39e5a1f0158
出典データセット
uspto-grants-1980_09
特許番号
US04221910

反応ノート

読み込み中…