Hydrochloric Acid → 3-Chloro-N-{2-methyl-3-[3-(methyloxy)phenyl]-6-oxo-6,7-dihydrothieno[2,3-b]pyridin-4-yl}benzenesulfonamide

HRID 573689ノート

反応式

HRID 573689 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([O:18]C)[N:15]=[C:14]3[S:20][C:21]([CH3:31])=[C:22]([C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[CH:24]=4)[C:13]=23)(=[O:10])=[O:9])[CH:5]=[CH:6][CH:7]=1.Cl>CO>[Cl:1][C:2]1[CH:3]=[C:4]([S:8]([NH:11][C:12]2[C:13]3[C:22]([C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[CH:24]=4)=[C:21]([CH3:31])[S:20][C:14]=3[NH:15][C:16](=[O:18])[CH:17]=2)(=[O:9])=[O:10])[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 683237633-Chloro-N-{2-methyl-6-(methyloxy)-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridin-4-yl}benzenesulfonamide

生成物 1

HCID 683238243-Chloro-N-{2-methyl-3-[3-(methyloxy)phenyl]-6-oxo-6,7-dihydrothieno[2,3-b]pyridin-4-yl}benzenesulfonamide収率 61.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 3-chloro-N-{2-methyl-6-(methyloxy)-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridin-4-yl}benzenesulfonamide (Example 115) (98 mg, 0.206 mmol) in 37% HCl (2 mL, 24.35 mmol) was heated to 100° C. under nitrogen atmosphere overnight. The reaction mixture was cooled to RT, diluted with MeOH and concentrated in vacuo. The residue was purified by MDAP (acidic conditions), to afford the title compound (58 mg). LCMS (A) m/z: 461 [M+1]+, Rt 1.27 min (acidic).

後処理

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified by MDAP (acidic conditions)

出典と根拠

ORDレコード
ord-7c2a0a19392e407a89c55d58db8ba1de
出典データセット
uspto-grants-2015_05
特許番号
US09029545B2

反応ノート

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