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Trifluoroacetic acid → URAT1 inhibitor 8

HRID 2178114
ノート
印刷プレビュー

反応式

HRID 2178114 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([OH:10])[CH:5]=[CH:6][C:7]=1[CH2:8][OH:9].[C:11]([C:13]1[CH:14]=[C:15]([S:20]([N:23](CC2C=CC(OC)=CC=2OC)[C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][N:25]=2)(=[O:22])=[O:21])[CH:16]=[CH:17][C:18]=1F)#[N:12].C(=O)([O-])[O-].[K+].[K+].C(O)(C(F)(F)F)=O>CS(C)=O.C(Cl)Cl.CO.CCOC(C)=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[CH2:8][OH:9])[O:10][C:18]1[CH:17]=[CH:16][C:15]([S:20]([NH:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][N:25]=2)(=[O:21])=[O:22])=[CH:14][C:13]=1[C:11]#[N:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 212878153-Chloro-4-(hydroxymethyl)phenolHCID 1176533623-cyano-N-(2,4-di methoxybenzyl)-4-fluoro-N-(5-fluoropyridin-2-yl)benzenesulfonamide

生成物 1

HCID 86271138URAT1 inhibitor 8収率 26.2%

試薬・触媒・溶媒 5

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution of 3-chloro-4-(hydroxymethyl)phenol (120 mg, 0.54 mmol) and 3-cyano-N-(2,4-di methoxybenzyl)-4-fluoro-N-(5-fluoropyridin-2-yl)benzenesulfonamide (Preparation 18, 100 mg, 0.22 mmol) in DMSO (1.5 mL) was added potassium carbonate (78 mg, 0.56 mmol) and the reaction stirred at room temperature for 72 hours. Water (10 mL) and EtOAc (15 mL) were added and the layers separated. The aqueous phase was extracted with EtOAc. The combined organic extracts were washed with brine, dried over magnesium sulphate and concentrated in vacuo. The crude product was purified by silica gel column chromatography eluting with 3:2 EtOAc:heptanes. The residue (76 mg, 0.13 mmol) was dissolved in DCM (2 mL) and treated with TFA (2 mL). The reaction was stirred at room temperature for 18 hours. MeOH (1 mL) was added and the reaction concentrated in vacuo. The crude product was purified by silica gel column chromatography eluting with 10-30% EtOAc in DCM to afford the title compound (25 mg, 44%) as a colourless solid (25 mg, 44%).

後処理

  1. customthe layers separated
  2. extractionThe aqueous phase was extracted with EtOAc
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by silica gel column chromatography
  7. washeluting with 3:2 EtOAc
  8. stirringThe reaction was stirred at room temperature for 18 hours
  9. concentrationthe reaction concentrated in vacuo
  10. customThe crude product was purified by silica gel column chromatography
  11. washeluting with 10-30% EtOAc in DCM

出典と根拠

ORDレコード
ord-54adccfd4a814341b5ef42bbcb43ad51
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09067922B2

反応ノート

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