Lithium Hydroxide → HCID 66893063、化合物

HRID 19267ノート

反応式

HRID 19267 の反応式
C[O:2][C:3](=[O:26])[C@@H:4]([N:12]1[CH2:16][C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)=[CH:14][C:13]1=[O:25])[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[OH-].[Li+]>O1CCCC1.O>[Cl:24][C:20]1[CH:19]=[C:18]([CH:23]=[CH:22][CH:21]=1)[O:17][C:15]1[CH2:16][N:12]([C@@H:4]([CH2:5][CH:6]2[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[C:3]([OH:26])=[O:2])[C:13](=[O:25])[CH:14]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 66894516(S)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid methyl ester

生成物 1

HCID 66893063HCID 66893063、化合物収率 86%

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

反応条件

温度
23 °C

実験手順

To a stirred solution of (S)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid methyl ester (340 mg, 0.9 mmol) in tetrahydrofuran-water (3:1, 10 mL) was added lithium hydroxide (118 mg, 2.7 mmol). The reaction mixture was stirred at 23° C. for 2 h. After this time, the mixture was concentrated and the reaction mixture was diluted with water. The reaction mixture was acidified with 2N hydrochloric acid, during which time precipitation occurred. The precipitate was removed by filtration, washed with cold water and dried in vacuo to obtain (S)-2-[4-(3-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-3-cyclohexyl-propionic acid (280 mg, 86%) as an off-white solid.

後処理

  1. concentrationAfter this time, the mixture was concentrated
  2. additionthe reaction mixture was diluted with water
  3. customThe reaction mixture was acidified with 2N hydrochloric acid, during which time precipitation
  4. customThe precipitate was removed by filtration
  5. washwashed with cold water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-bf470c71001d4023b15de42f30ce4a1d
出典データセット
uspto-grants-2010_06
特許番号
US07741327B2

反応ノート

読み込み中…