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Hydrochloric Acid → 6-Amino-5-[(6-hydroxy-2,5,7,8-tetramethyl-2-chromanylmethyl)amino]-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione

HRID 399424
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HRID 399424 반응식
C([O:4][C:5]1[C:6]([CH3:37])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][C:10]([CH3:36])([C:17]([NH:19][C:20]1[C:21](=[O:35])[N:22]([CH3:34])[C:23](=[O:33])[N:24]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:25]=1[NH2:26])=O)[CH2:9][CH2:8]2)(=O)C.Cl>C1COCC1>[NH2:26][C:25]1[N:24]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:23](=[O:33])[N:22]([CH3:34])[C:21](=[O:35])[C:20]=1[NH:19][CH2:17][C:10]1([CH3:36])[CH2:9][CH2:8][C:7]2[C:12](=[C:13]([CH3:16])[C:14]([CH3:15])=[C:5]([OH:4])[C:6]=2[CH3:37])[O:11]1
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참가 물질

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HCID 313Hydrochloric AcidHCID 572790375-(6-Acetoxy-2.5,7,8-tetramethvlchroman-2-carboxamido)-6-amino-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione

생성물 1

HCID 1317208806-Amino-5-[(6-hydroxy-2,5,7,8-tetramethyl-2-chromanylmethyl)amino]-3-methyl-1-phenyl-2,4 (1H, 3H)-pyrimidinedione수율 35%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The compound of Example 14 (64 mg, 1.0 mmol) was dissolved in THF (10 mL). To the resultant solution was added borane-methyl sulfide complex (10 M, 0.24 mL, 2.4 mmol). The resultant reaction mixture was refluxed for 5 h. To the resultant was added 1N hydrochloric acid (2.4 mL) under ice-cooling. The resultant mixture was refluxed for 2 h, followed by concentration under reduced pressure. The residue was extracted with dichloromethane after addition of 1N aqueous solution of sodium hydroxide. The organic layer was washed with 10% aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was crystallized by addition of ethyl acetate and ether to give the title compound (yield 35%).

후처리

  1. customThe resultant reaction mixture
  2. temperaturewas refluxed for 5 h
  3. temperaturecooling
  4. concentrationfollowed by concentration under reduced pressure
  5. extractionThe residue was extracted with dichloromethane
  6. additionafter addition of 1N aqueous solution of sodium hydroxide
  7. washThe organic layer was washed with 10% aqueous solution of sodium chloride
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was crystallized by addition of ethyl acetate and ether

출처 및 근거

ORD 기록
ord-706e3c1f043d4f1c82e5b7ec86c93210
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05821247

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