Lithium hydroxide, monohydrate → HCID 71226525、化合物

HRID 713449ノート

反応式

HRID 713449 の反応式
C([O:3][C:4](=[O:24])[CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([C:12](=[O:23])[C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=2)[CH2:8][CH2:7]1)C.O[Li].O>>[CH3:22][O:21][C:15]1[CH:14]=[C:13]([CH:18]=[CH:17][C:16]=1[O:19][CH3:20])[C:12]([CH:9]1[CH2:8][CH2:7][N:6]([CH2:5][C:4]([OH:24])=[O:3])[CH2:11][CH2:10]1)=[O:23]

参加物

3

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 71226849[4-(3,4-Dimethoxy-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester

生成物 1

HCID 71226525HCID 71226525、化合物収率 92.5%

実験手順

To a solution of [4-(3,4-dimethoxy-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester (0.45 g, 1.34 mmol in 6 mL of THF and 2 mL of methanol) was added LiOH.H2O (0.28 g, 6.7 mmol in 3 mL of water) and the reaction mixture was stirred at ambient temperature for 1.5 hours. The solvent was removed in vacuo then diluted with 20 mL of water (pH 14). The residue was treated with 12 mL of 1 N HCl (pH 4), frozen at −78° C. and lyophilized for 24 hours to yield the title compound (0.40 g, 1.24 mmol). MS (ESI) m/z 308.3 (M+H+); HPLC (Novapak 150×3.9 mm C-18 column: mobile phase: 35-90% acetonitrile/water with 0.1% TFA, at 2 mL/min over 2 min.) t 1.16 min.

後処理

  1. customThe solvent was removed in vacuo
  2. additionthen diluted with 20 mL of water (pH 14)
  3. additionThe residue was treated with 12 mL of 1 N HCl (pH 4)
  4. temperaturefrozen at −78° C.
  5. waitlyophilized for 24 hours

出典と根拠

ORDレコード
ord-be4eb5b839184aa59b71d2b78d54024a
出典データセット
uspto-grants-2015_11
特許番号
US09181266B2

反応ノート

読み込み中…