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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
ノート
印刷プレビュー

反応式

HRID 539250 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒

2
HCID 887Methanol溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
53 °C

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-8d15dc91050643dc93b703494b74a80f
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865896B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート