HCID 21998633, 화합물 → HCID 9822510, 화합물

HRID 1976563노트

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HRID 1976563 반응식
[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

참가 물질

4

반응물 1

HCID 21998633HCID 21998633, 화합물

생성물 1

HCID 9822510HCID 9822510, 화합물수율 75.5%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 10311-Propanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-3da6cae8d807459bb8d9d432ca4a3c20
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06228859B1

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