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Chloroform → 6-Amino-2-butoxy-9-{3-[(3-morpholin-4-ylpropyl)amino]propyl}-7,9-dihydro-8H-purine-8-one dimaleate

HRID 539250
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HRID 539250 반응식
Cl.Cl.Cl.[NH2:4][C:5]1[N:13]=[C:12]([O:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:11]=[C:10]2[C:6]=1[NH:7][C:8](=[O:32])[N:9]2[CH2:19][CH2:20][CH2:21][NH:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1.C(=O)([O-])[O-].[Na+].[Na+].C(Cl)(Cl)Cl.[C:43]([OH:50])(=[O:49])/[CH:44]=[CH:45]\[C:46]([OH:48])=[O:47]>[Cl-].[Na+].O.CO>[C:43]([OH:50])(=[O:49])/[CH:44]=[CH:45]\[C:46]([OH:48])=[O:47].[C:43]([OH:50])(=[O:49])/[CH:44]=[CH:45]\[C:46]([OH:48])=[O:47].[NH2:4][C:5]1[N:13]=[C:12]([O:14][CH2:15][CH2:16][CH2:17][CH3:18])[N:11]=[C:10]2[C:6]=1[NH:7][C:8](=[O:32])[N:9]2[CH2:19][CH2:20][CH2:21][NH:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:27][CH2:28][O:29][CH2:30][CH2:31]1
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참가 물질

7

반응물 4

HCID 6212ChloroformHCID 10340Sodium CarbonateHCID 444266Maleic AcidHCID 669632426-amino-2-butoxy-9-{3-[(3-morpholin-4-ylpropyl)amino]propyl}-7,9-dihydro-8H-purine-8-one trihydrochloride

생성물 1

HCID 866513626-Amino-2-butoxy-9-{3-[(3-morpholin-4-ylpropyl)amino]propyl}-7,9-dihydro-8H-purine-8-one dimaleate수율 94.8%

시약·촉매·용매

2
HCID 887Methanol용매HCID 57417360Sodium chloride; water용매

반응 조건

온도
53 °C

실험 절차

To a solution of 6-amino-2-butoxy-9-{3-[(3-morpholin-4-ylpropyl)amino]propyl}-7,9-dihydro-8H-purine-8-one trihydrochloride (15.00 g, 29.02 mmol) in 10% brine (105.00 g) was added an aqueous 10% sodium carbonate to be neutralized. After adding chloroform (335.7 g), the mixture was heated to 53° C., and the aqueous layer was separated and removed. After an organic layer was concentrated, to the residue was added methanol (296.63 g) and the mixture was raised to 50° C. After methanol (59.33 g) containing maleic acid (6.74 g, 58.04 mmol) was dropped, a white crystal was confirmed. After stirring at 70° C. for 1 hour, the mixture was cooled to 5° C., a crystal was filtered, washed and dried to give the subject compound (17.60 g, 94.8%). Purity: 99.62% (HPLC)

후처리

  1. customthe aqueous layer was separated
  2. customremoved
  3. concentrationAfter an organic layer was concentrated, to the residue
  4. additionwas added methanol (296.63 g)
  5. temperaturethe mixture was raised to 50° C
  6. additionwas dropped
  7. temperaturethe mixture was cooled to 5° C.
  8. filtrationa crystal was filtered
  9. washwashed
  10. customdried

출처 및 근거

ORD 기록
ord-8d15dc91050643dc93b703494b74a80f
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865896B2

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