Hydrochloric Acid → HCID 56601188、化合物

HRID 1619603ノート

反応式

HRID 1619603 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:8]=[C:9]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH:10]=[CH:11][C:12]=2[OH:13])=[CH:5][CH:4]=[N:3]1.[C:20]([C:22]1[CH:23]=[C:24]([S:29]([NH:32][C:33]2[CH:38]=[CH:37][C:36]([F:39])=[CH:35][N:34]=2)(=[O:31])=[O:30])[CH:25]=[CH:26][C:27]=1F)#[N:21].C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[C:20]([C:22]1[CH:23]=[C:24]([S:29]([NH:32][C:33]2[CH:38]=[CH:37][C:36]([F:39])=[CH:35][N:34]=2)(=[O:30])=[O:31])[CH:25]=[CH:26][C:27]=1[O:13][C:12]1[CH:11]=[CH:10][C:9]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[CH:8][C:7]=1[C:6]1[N:2]([CH3:1])[N:3]=[CH:4][CH:5]=1)#[N:21]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 594366003-cyano-4-fluoro-N-(5-fluoropyridin-2-yl)benzenesulfonamideHCID 1362008913-(1-methyl-1H-pyrazol-5-yl)biphenyl-4-ol

生成物 1

HCID 56601188HCID 56601188、化合物収率 18%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

In a pressure sealed vial, 3-(1-methyl-1H-pyrazol-5-yl)biphenyl-4-ol (Preparation 107, mg, 0.19 mmol), 3-cyano-4-fluoro-N-(5-fluoropyridin-2-yl)benzenesulfonamide (WO2010079443, 50 mg, 0.17 mmol) and potassium carbonate (70 mg, 0.51 mmol) were stirred at 90° C. in dimethyl sulfoxide for 18 hours. The mixture was cooled down to room temperature and treated with 2M hydrochloric acid (5 mL). The mixture was stirred for 1 hour and the resulting precipitate was filtered and purified by preparative HPLC to afford the title compound (17 mg, 18%) as a white solid.

後処理

  1. customIn a pressure sealed vial
  2. filtrationthe resulting precipitate was filtered
  3. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-b11b70dbe51f41ae965e70c0258030aa
出典データセット
uspto-grants-2014_07
特許番号
US08772293B2

反応ノート

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