Sodium Hydroxide → HCID 21978853、化合物

HRID 729385ノート

反応式

HRID 729385 の反応式
C([O:3][C:4](=[O:21])[C:5]1[CH:10]=[C:9]([F:11])[C:8]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)=[CH:7][C:6]=1[NH:17][CH:18]1[CH2:20][CH2:19]1)C.[OH-].[Na+]>CO.O1CCCC1.C(OCC)(=O)C>[CH:18]1([NH:17][C:6]2[CH:7]=[C:8]([N:12]3[CH2:13][CH2:14][CH2:15][CH2:16]3)[C:9]([F:11])=[CH:10][C:5]=2[C:4]([OH:21])=[O:3])[CH2:19][CH2:20]1

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 210411862-Cyclopropylamino-5-fluoro-4-pyrrolidin-1-ylbenzoic acid ethyl ester

生成物 1

HCID 21978853HCID 21978853、化合物収率 89.9%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a solution of 4-(pyrrolidin-1-yl)-2-cyclopropylamino-5-fluorobenzoic acid ethyl ester (Example 3e, 3.10 g, 10.4 mmol) in methanol (50 mL) and tetrahydrofuran (20 mL) is added 1N solution of sodium hydroxide (35 mL). The reaction mixture is stirred at 80° C. for 20 hours, cooled to room temperature, and diluted with ethyl acetate. The organic layer is washed with 1N hydrochloric acid, water, and brine. The organic layer is dried over MgSO4, filtered, and the filtrate concentrated to afford the title compound as a solid (2.47 g). MS CI: m/z 263 (M+).

後処理

  1. temperaturecooled to room temperature
  2. washThe organic layer is washed with 1N hydrochloric acid, water, and brine
  3. dry with materialThe organic layer is dried over MgSO4
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated

出典と根拠

ORDレコード
ord-9ea1d6cf80ca43d3ada89f06678035c4
出典データセット
uspto-grants-2009_09
特許番号
US07582627B2

反応ノート

読み込み中…