Sodium Hydroxide → 2-(4-BOC-PIPERAZINYL)-2-PHENYLACETIC ACID

HRID 1376029노트

반응식

HRID 1376029 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH:14]([C:21]([O:23]C)=[O:22])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>CCO>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([CH:14]([C:21]([OH:23])=[O:22])[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 23386132Tert-butyl 4-(2-methoxy-2-oxo-1-phenylethyl)piperazine-1-carboxylate

생성물 1

HCID 27622172-(4-BOC-PIPERAZINYL)-2-PHENYLACETIC ACID수율 86.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 4-(Methoxycarbonyl-phenyl-methyl)-piperazine-1-carboxylic acid tert-butyl ester (151) (30.4 g, 87.25 mmol) in EtOH (200 mL) was added of 1N NaOH (192 mL) and the reaction mixture was allowed to stir at room temperature for 18 h. The reaction mixture is then concentrated to dryness. The resulting residue is taken up in H2O and acidified slowly at 0° C. with 10% NaSO4 (pH=5–6). The desired product was then extracted into EtOAc. The organic phase was then concentrated to dryness yielding 24.3 g (86%) product.

후처리

  1. concentrationThe reaction mixture is then concentrated to dryness
  2. customacidified slowly at 0° C. with 10% NaSO4 (pH=5–6)
  3. extractionThe desired product was then extracted into EtOAc
  4. concentrationThe organic phase was then concentrated to dryness

출처 및 근거

ORD 기록
ord-be94f9d76e8f41ebb907bb3e24e6e3e8
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07169777B2

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