Hydrochloric Acid → HCID 68528052、化合物

HRID 1723845

反応式

HRID 1723845 の反応式
C(O[C:6]([N:8]1[CH2:13][CH2:12][CH2:11][C:10]([CH:15]([O:23][C:24]2[C:32]3[C:27](=[CH:28][CH:29]=[C:30]([F:33])[CH:31]=3)[NH:26][N:25]=2)C2C=CC=CC=2F)(C)[CH2:9]1)=O)(C)(C)C.[ClH:34]>CCOC(C)=O.O1CCOCC1>[ClH:34].[F:33][C:30]1[CH:31]=[C:32]2[C:27](=[CH:28][CH:29]=1)[N:26]([C:29]1[CH:28]=[CH:27][CH:32]=[CH:31][C:30]=1[F:33])[N:25]=[C:24]2[O:23][CH2:15][CH:10]1[CH2:11][CH2:12][CH2:13][N:8]([CH3:6])[CH2:9]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 685314413-[5-fluoro-1-(2-fluoro-phenyl)-1H-indazol-3-yloxymethyl]-3-methyl-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 68528052HCID 68528052、化合物収率 81.7%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a room temperature stirred solution of Intermediate 57 (0.127 g, 0.278 mmol) in EtOAc (0.925 ml) was added 0.902 ml of a 4.0 M HCl solution in dioxane. The reaction was allowed to stir overnight at room temperature. Upon completion as indicated by HPLC, the reaction was concentrated under reduced pressure. EtOAc was added to the solid and then concentrated down under reduced pressure. This process was repeated five times. The solid was triturated with EtOAc/Et2O (2:1), the solid was filtered and then washed with Et2O (2×15 ml). The solid was placed in a drying oven under reduced pressure to yield 0.089 g (81.7%) of the title product.

後処理

  1. concentrationthe reaction was concentrated under reduced pressure
  2. additionEtOAc was added to the solid
  3. concentrationconcentrated down under reduced pressure
  4. customThe solid was triturated with EtOAc/Et2O (2:1)
  5. filtrationthe solid was filtered
  6. washwashed with Et2O (2×15 ml)
  7. customThe solid was placed in a drying oven under reduced pressure

出典と根拠

ORDレコード
ord-c724f911d65e4b85b580490b9a32eb1c
出典データセット
uspto-grants-2009_02
特許番号
US07485636B2

関連ノート

読み込み中…