Lithium hydroxide, monohydrate → HCID 10370074, 화합물

HRID 965643

반응식

HRID 965643 반응식
C([O:3][C:4]([CH:6]1[CH2:11][N:10]([CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8][N:7]1[C:25](=[O:40])[CH2:26][CH:27]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:5])C.O[Li].O>C1COCC1.CO.O>[CH:12]([N:10]1[CH2:9][CH2:8][N:7]([C:25](=[O:40])[CH2:26][CH:27]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:6]([C:4]([OH:5])=[O:3])[CH2:11]1)([C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 103247844-Benzhydryl-1-(3,3-diphenyl-propionyl)-piperazine-2-carboxylic acid ethyl ester

생성물 1

HCID 10370074HCID 10370074, 화합물수율 95%

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

A mixture of 4-Benzhydryl-1-(3,3-diphenyl-propionyl)-piperazine-2-carboxylic acid ethyl ester (0.51 g, 0.957 mmol), and LiOH.H2O (0.12 g, 2.87 mmol) in THF/MeOH/H2O (15:5:5) was stirred at room temperature for two days. The solvent was evaporated under reduced pressure, the residue was dissolved in water, acidified with 1N HCl to pH 3. The product was extracted with EtOAc, dried with MgSO4, and evaporated under reduced pressure. The product was purified by column chromatography (CH2Cl2:MeOH 15:1) to give the title compound in 95% yield.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in water
  3. extractionThe product was extracted with EtOAc
  4. dry with materialdried with MgSO4
  5. customevaporated under reduced pressure
  6. customThe product was purified by column chromatography (CH2Cl2:MeOH 15:1)

출처 및 근거

ORD 기록
ord-c25aec51b3fa40519e670da4c9954493
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06951862B2

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