Hydrochloric Acid → N-Cyclopropyl-3-fluoro-5-(1H-indazol-5-yl)-4-methylbenzamide

HRID 1988931ノート

反応式

HRID 1988931 の反応式
[CH:1]1([NH:4][C:5]([C:7]2[CH:8]=[C:9]([F:30])[C:10]([CH3:29])=[C:11]([C:13]3[CH:14]=[C:15]4[C:19](=[CH:20][CH:21]=3)[N:18](C(OC(C)(C)C)=O)[N:17]=[CH:16]4)[CH:12]=2)=[O:6])[CH2:3][CH2:2]1.Cl>O1CCOCC1>[CH:1]1([NH:4][C:5](=[O:6])[C:7]2[CH:12]=[C:11]([C:13]3[CH:14]=[C:15]4[C:19](=[CH:20][CH:21]=3)[NH:18][N:17]=[CH:16]4)[C:10]([CH3:29])=[C:9]([F:30])[CH:8]=2)[CH2:2][CH2:3]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59127378HCID 59127378、化合物

生成物 1

HCID 10403067N-Cyclopropyl-3-fluoro-5-(1H-indazol-5-yl)-4-methylbenzamide収率 17.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 1,1-dimethylethyl 5-{5-[(cyclopropylamino)carbonyl]-3-fluoro-2-methylphenyl}-1H-indazole-1-carboxylate (Example 59) (0.46 g) in a solution of hydrogen chloride in dioxan (4M, 7 ml) was stirred at room temp. under nitrogen for 4.5 h. The solvent was evaporated and the residue was partitioned between dichloromethane (20 ml) and aqueous sodium hydroxide (2M, 20 ml). The organic layer was separated using a hydrophobic filter tube, the solvent was evaporated and the residue was purified on a Varian Bond-Elut SPE cartridge (silica, 10 g) eluting with chloroform:methanol (100:0 to 98:2) to give the title compound (0.06 g).

後処理

  1. customThe solvent was evaporated
  2. customthe residue was partitioned between dichloromethane (20 ml) and aqueous sodium hydroxide (2M, 20 ml)
  3. customThe organic layer was separated
  4. customthe solvent was evaporated
  5. customthe residue was purified on a Varian Bond-Elut SPE cartridge (silica, 10 g)
  6. washeluting with chloroform:methanol (100:0 to 98:2)

出典と根拠

ORDレコード
ord-4a4e7dda642744afbed03239ed0464b9
出典データセット
uspto-grants-2010_01
特許番号
US07642276B2

反応ノート

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