HCID 21998633、化合物 → HCID 9822510、化合物

HRID 1976563ノート

反応式

HRID 1976563 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:27]=[CH:28][C:29]=1[O:30][CH3:31])[CH2:12][N:13]1[C:21]2[N:20]=[C:19]([CH:22]([CH3:24])[CH3:23])[NH:18][C:17]=2[C:16](=[O:25])[NH:15][C:14]1=S)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)CC.[Ni]>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:27]=[CH:28][C:29]=1[O:30][CH3:31])[CH2:12][N:13]1[C:21]2[N:20]=[C:19]([CH:22]([CH3:24])[CH3:23])[NH:18][C:17]=2[C:16](=[O:25])[N:15]=[CH:14]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 21998633HCID 21998633、化合物

生成物 1

HCID 9822510HCID 9822510、化合物収率 75.5%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 10311-Propanol溶媒

実験手順

3-(3-Benzyloxy-4-methoxy-benzyl)-8-isopropyl-2-thioxanthine (21.83 g, 50 mmole) was heated under reflux in 1-propanol (700 ml) with Raney-nickel (30 g) (pre-treated with 0.1% of aqueous acetic acid). After 4 hours the nickel was filtered off and washed with hot propanol and chloroform. The solution was evaporated to dryness in vacuo. The residue was dissolved in chloroform, extracted with IM sodium carbonate solution, dried (Na2SO4), treated twice with charcoal (0.8 g), filtered and evaporated to dryness in vacuo. The residue was suspended in hot acetone (250 ml), concentrated and the solid collected at 0-5° C. to give 3-(3-benzyloxy-4-methoxy-benzyl)-8-isopropyl-hypoxanthine (15.27 g, 75.5%), mp 233-235° C.

後処理

  1. filtrationAfter 4 hours the nickel was filtered off
  2. washwashed with hot propanol and chloroform
  3. customThe solution was evaporated to dryness in vacuo
  4. dissolutionThe residue was dissolved in chloroform
  5. extractionextracted with IM sodium carbonate solution
  6. dry with materialdried (Na2SO4)
  7. additiontreated twice with charcoal (0.8 g)
  8. filtrationfiltered
  9. customevaporated to dryness in vacuo
  10. concentrationconcentrated
  11. customthe solid collected at 0-5° C.

出典と根拠

ORDレコード
ord-3da6cae8d807459bb8d9d432ca4a3c20
出典データセット
uspto-grants-2001_05
特許番号
US06228859B1

反応ノート

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