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Lithium Hydroxide → 4-[4-(4-Tert-butylphenyl)-piperazin-1-yl]-butyric acid lithium salt

HRID 511203
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반응식

HRID 511203 반응식
C([O:3][C:4](=[O:24])[CH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)C.[OH-].[Li+:26].C(#N)C>O1CCCC1>[Li+:26].[C:20]([C:17]1[CH:16]=[CH:15][C:14]([N:11]2[CH2:10][CH2:9][N:8]([CH2:7][CH2:6][CH2:5][C:4]([O-:24])=[O:3])[CH2:13][CH2:12]2)=[CH:19][CH:18]=1)([CH3:23])([CH3:21])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 6342AcetonitrileHCID 585764584-[4-(4-Tert-butyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

생성물 1

HCID 585763684-[4-(4-Tert-butylphenyl)-piperazin-1-yl]-butyric acid lithium salt수율 189.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 4-[4-(4-tert-butyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester (1.41 g; 4.24 mmol, prepared in accordance with Example 166) is added a solution of lithium hydroxide (59 mg; 2.46 mmol in 3 mL of water) diluted with tetrahydrofuran (3 mL) and the resulting mixture is stirred at room temperature for one hour. Acetonitrile (50 mL) is added and the precipitate formed is then filtered and dried under high vacuum to afford the desired product (1.45 g) which is used in the next step without further purification.

후처리

  1. customthe precipitate formed
  2. filtrationis then filtered
  3. customdried under high vacuum

출처 및 근거

ORD 기록
ord-c01460ba21404059891c2a309082a073
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096524B2

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