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Hydrochloric Acid → 2-(4-Methoxy-phenyl)-6-[3-methoxy-4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-5,6-dihydro-4h-thieno[2,3-c]pyridin-7-one, hydrochloride

HRID 2384881
ノート
印刷プレビュー

反応式

HRID 2384881 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:18][C:12]3[C:13](=[O:17])[NH:14][CH2:15][CH2:16][C:11]=3[CH:10]=2)=[CH:5][CH:4]=1.Br[C:20]1[CH:33]=[CH:32][C:23]([O:24][CH2:25][CH2:26][N:27]2[CH2:31][CH2:30][CH2:29][CH2:28]2)=[C:22]([O:34][CH3:35])[CH:21]=1.CNCCNC.C([O-])([O-])=O.[K+].[K+].[ClH:48].CCO>C1(C)C=CC=CC=1.CCOC(C)=O.CO.[Cu]I>[ClH:48].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:18][C:12]3[C:13](=[O:17])[N:14]([C:20]4[CH:33]=[CH:32][C:23]([O:24][CH2:25][CH2:26][N:27]5[CH2:28][CH2:29][CH2:30][CH2:31]5)=[C:22]([O:34][CH3:35])[CH:21]=4)[CH2:15][CH2:16][C:11]=3[CH:10]=2)=[CH:5][CH:4]=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 313Hydrochloric AcidHCID 702EthanolHCID 8070N,N'-DimethylethylenediamineHCID 11430Potassium CarbonateHCID 229943381-[2-(4-Bromo-2-methoxyphenoxy)ethyl]pyrrolidineHCID 576495112-(4-Methoxy-phenyl)-5,6-dihydro-4H-thieno[2,3-c]pyridin-7-one

生成物 1

HCID 24803081
2-(4-Methoxy-phenyl)-6-[3-methoxy-4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-5,6-dihydro-4h-thieno[2,3-c]pyridin-7-one, hydrochloride
収率 100%

試薬・触媒・溶媒 4

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Combine 2-(4-methoxy-phenyl)-5,6-dihydro-4H-thieno[2,3-c]pyridin-7-one (0.234 g, 0.90 mmol), 1-[2-(4-bromo-2-methoxy-phenoxy)-ethyl]-pyrrolidine (Bastian, J. A., et al WO 9725033 A1) (0.271 g, 0.90 mmol), N,N′-dimethyl-ethane-1,2-diamine (16 mg, 0.18 mmol), K2CO3 (0.249 g, 1.81 mmol), and CuI (17 mmol, 0.09 mmol) in toluene (10 mL) and stir at 110° C. for 48 h. Dilute with EtOAc (100 mL) and wash with water (50 mL), containing NH3—H2O (5 mL) three times. Dry over Na2SO4, filter and purify the material by chromatography, eluting with 7% 2 M NH3 in CH3OH, and 93% CH2Cl2 to give 0.125 g. Dissolve the material in CH3OH (5 mL) and treat with 1.0 M HCl in EtOH (270 μL, 0.27 mmol). Stir at RT for 5 min and concentrate to give the title compound (0.133 g, 0.26 mmol, 100%). LC-MS/ES m/z 479.3 [M+H]+.

後処理

  1. washwash with water (50 mL)
  2. additioncontaining NH3—H2O (5 mL) three times
  3. dry with materialDry over Na2SO4
  4. filtrationfilter
  5. custompurify the material by chromatography
  6. washeluting with 7% 2 M NH3 in CH3OH, and 93% CH2Cl2
  7. customto give 0.125 g
  8. concentrationconcentrate

出典と根拠

ORDレコード
ord-7b7873e97f424edf85cd0566cf867cf3
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263772B2

反応ノート

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