Lithium hydroxide, monohydrate → HCID 71226525, 화합물

HRID 713449노트

반응식

HRID 713449 반응식
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]

참가 물질

3

반응물 2

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

생성물 1

HCID 71226525HCID 71226525, 화합물수율 92.5%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-be4eb5b839184aa59b71d2b78d54024a
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181266B2

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