Stannous Chloride → N-(3-amino-4-(1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)phenyl)-4-chlorobenzamide

HRID 530774

反応式

HRID 530774 の反応式
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[N:19]([CH3:20])[N:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=3)=[C:11]([N+:25]([O-])=O)[CH:10]=2)=[O:7])=[CH:4][CH:3]=1.[Sn](Cl)Cl>CO>[NH2:25][C:11]1[CH:10]=[C:9]([NH:8][C:6](=[O:7])[C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:29][CH:28]=2)[CH:14]=[CH:13][C:12]=1[C:15]1[N:19]([CH3:20])[N:18]=[C:17]([C:21]([F:24])([F:22])[F:23])[CH:16]=1

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 674670954-chloro-N-(4-(1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)-3-nitrophenyl)benzamide

生成物 1

HCID 67464229N-(3-amino-4-(1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)phenyl)-4-chlorobenzamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Compound 16 (42 mg, 0.1 mmol) was dissolved in 10 ml MeOH. Tin(II)chloride dehydrate (223 mg, 1 mmol) was added and the reaction mixture was stirred at r.t. for overnight. The reaction mixture was evaporated to dryness. The solid residue was dissolved in 6 N NaOH and extracted with DCM. The org. phase was washed with brine. After concentrated to dryness, the solid residue was dissolved in DMF and purified on prep HPLC to give compound 17.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionThe solid residue was dissolved in 6 N NaOH
  3. extractionextracted with DCM
  4. washphase was washed with brine
  5. concentrationAfter concentrated to dryness
  6. dissolutionthe solid residue was dissolved in DMF
  7. custompurified on prep HPLC

出典と根拠

ORDレコード
ord-b040b2b233b145f481e1f95e6bcfc3d0
出典データセット
uspto-grants-2016_05
特許番号
US09353099B2

関連ノート

読み込み中…