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Acetone → HCID 44198125、化合物

HRID 79619
ノート
印刷プレビュー

反応式

HRID 79619 の反応式
[NH2:1][CH2:2][CH2:3][C:4]([N:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:17]([Br:18])=[CH:16][N:15]=[C:14]3[NH:19][CH:20]=[C:21]([NH:22][C:23](=[O:30])[C:24]4[CH:29]=[CH:28][CH:27]=[N:26][CH:25]=4)[C:13]=23)[CH2:8][CH2:7]1)=[O:5].[CH3:31][C:32]([CH3:34])=O.CCN(C(C)C)C(C)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+].Cl>C(Cl)Cl.CCOCC.CN(C=O)C.ClCCCl>[Br:18][C:17]1[C:12]([N:9]2[CH2:8][CH2:7][N:6]([C:4](=[O:5])[CH2:3][CH2:2][NH:1][CH:32]([CH3:34])[CH3:31])[CH2:11][CH2:10]2)=[C:13]2[C:21]([NH:22][C:23](=[O:30])[C:24]3[CH:29]=[CH:28][CH:27]=[N:26][CH:25]=3)=[CH:20][NH:19][C:14]2=[N:15][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 44198124N-(4-(4-(3-aminopropanoyl)piperazin-1-yl)-5-bromo-1H-pyrrolo[2,3-b]pyri din-3-yl)nicotinamide

生成物 1

HCID 44198125
HCID 44198125、化合物
収率 56.6%

試薬・触媒・溶媒 4

HCID 111,2-Dichloroethane溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

N-(4-(4-(3-aminopropanoyl)piperazin-1-yl)-5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)nicotinamide (0.060 g, 0.103 mmol, see Example 62) and acetone (0.0599 g, 1.03 mmol) were placed in 1:1 DCE:DMF (5 mL). DIEA (d 0.742; 0.0898 mL, 0.516 mmol) was then added, followed by the addition of NaBH(OAc)3 (0.0437 g, 0.206 mmol). The reaction was then stirred for 30 minutes, and poured into Na2CO3 and extracted into DCM (3×30 mL). The organic fractions were combined, dried, filtered and concentrated. The resulting residue was purified by reverse phase HPLC to give a pure product. The product was then dissolved in minimal DCM and added to a stirring solution of 1M HCl in ether (10 mL). The resulting solid was collected to give N-(5-bromo-4-(4-(3-(isopropylamino)propanoyl)piperazin-1-yl)-1H-pyrrolo[2,3-b]pyridin-3-yl)nicotinamide (0.030 g, 46.6% yield) as the trihydrochloride salt. MS APCI (+) m/z 515 detected.

後処理

  1. extractionextracted into DCM (3×30 mL)
  2. customdried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe resulting residue was purified by reverse phase HPLC
  6. customto give a pure product
  7. customThe resulting solid was collected

出典と根拠

ORDレコード
ord-0d7d6730ec534694ad6f2359f5cf163b
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841304B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート