Methane → HCID 18465367、化合物

HRID 437537

反応式

HRID 437537 の反応式
[CH2:1]([N:4]1[C:13](=[O:14])[C:12]2[NH:11][CH:10]=[N:9][C:8]=2[N:7]([CH2:15][CH2:16][CH3:17])[C:5]1=[O:6])[CH2:2][CH3:3].[OH-].[Na+].Cl[CH2:21][CH:22]([OH:25])[CH2:23][OH:24].C>O.C(O)(C)C.C(Cl)(Cl)Cl.CO>[OH:25][CH:22]([CH2:23][OH:24])[CH2:21][N:11]1[C:12]2[C:13](=[O:14])[N:4]([CH2:1][CH2:2][CH3:3])[C:5](=[O:6])[N:7]([CH2:15][CH2:16][CH3:17])[C:8]=2[N:9]=[CH:10]1

参加物

8

反応物 4

HCID 297MethaneHCID 72903-Chloro-1,2-propanediolHCID 14798Sodium HydroxideHCID 1693171,3-Dipropylxanthine

生成物 1

HCID 18465367HCID 18465367、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3776Isopropanol溶媒2 回HCID 21584188Chloroform methanol溶媒

実験手順

A suspension of 1,3-di-n-propylxanthine (250.1 g., 1.06 mole) in water (300 ml.) was treated with sodium hydroxide solution (50%, 85 ml.). The mixture was filtered, and evaporated to dryness. The residue obtained was treated with a solution of 1-chloro-2,3-dihydroxypropane (170 g., 1.59 mole) in isopropanol (700 ml.). The mixture was stirred at reflux overnight, filtered, and evaporated to dryness to obtain a brown gummy residue. This residue was dissolved in isopropyl alcohol, and stirred overnight with charcoal (20 gm.). The mixture was filtered, concentrated and allowed to crystallize over night at 0° to -5° C. The crystals were filtered, suspended in ether, refiltered and air dried to yield white crystals (224 g., 72.17%), melting point 88° - 91°. Tlc (5μl of a 5% solution) on a silica plate developed in chloroform:methanol (9.5:0.5) showed one spot. IR and NMR spectra were consistent with the proposed structure.

後処理

  1. filtrationThe mixture was filtered
  2. customevaporated to dryness
  3. customThe residue obtained
  4. temperatureat reflux overnight
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customto obtain a brown gummy residue
  8. filtrationThe mixture was filtered
  9. concentrationconcentrated
  10. customto crystallize over night at 0° to -5° C
  11. filtrationThe crystals were filtered
  12. customair dried
  13. customto yield white crystals (224 g., 72.17%), melting point 88° - 91°

出典と根拠

ORDレコード
ord-416bfc39d5184c4ca3f8be7fd02d440f
出典データセット
uspto-grants-1977_06
特許番号
US04031218

関連ノート

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