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Lithium Hydroxide → [7-(4-t-Butoxycarbonylpiperazin-1-yl)-3,4-dihydro-1(1H)-isoquinolinone-2-yl]acetic acid

HRID 1377525
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인쇄 미리보기

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HRID 1377525 반응식
C([O:3][C:4](=[O:30])[CH2:5][N:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][C:10]([N:16]3[CH2:21][CH2:20][N:19]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:18][CH2:17]3)=[CH:11][CH:12]=2)[C:7]1=[O:29])C.[Li+].[OH-]>CO>[C:25]([O:24][C:22]([N:19]1[CH2:18][CH2:17][N:16]([C:10]2[CH:9]=[C:8]3[C:13]([CH2:14][CH2:15][N:6]([CH2:5][C:4]([OH:30])=[O:3])[C:7]3=[O:29])=[CH:12][CH:11]=2)[CH2:21][CH2:20]1)=[O:23])([CH3:28])([CH3:26])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 10598069Ethyl [7-(4-t-butoxycarbonylpiperazin-1-yl)-3,4-dihydro-1(1H)-isoquinolinone-2-yl]acetate

생성물 1

HCID 11794693[7-(4-t-Butoxycarbonylpiperazin-1-yl)-3,4-dihydro-1(1H)-isoquinolinone-2-yl]acetic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Ethyl [7-(4-t-butoxycarbonylpiperazin-1-yl)-3,4-dihydro-1(1H)-isoquinolinone-2-yl]acetate (1-4) (2.9 g, 6.95 mmol), 1N LiOH (20.9 mL, 20.9 mmol) and MeOH (50 mL) were stirred for 16 hours at room temperature. The solvent was removed, the residue was taken up in EtOAc and washed with 1N HCl. Repeated extraction of the aqueous phase followed by washing of the bulked organic layers with brine (5 mL), drying (MgSO4) and evaporation afforded 1-5 as a solid. 1H NMR (CD3OD): d1.48 (9H, s), 2.99 (2H, t), 3.20 (4H, m), 3.62 (6H, m), 4.31 (2H, s), 7.22 (2H, s), 7.60 (1H, s).

후처리

  1. customThe solvent was removed
  2. washwashed with 1N HCl
  3. extractionextraction of the aqueous phase
  4. washby washing of the bulked organic layers with brine (5 mL)
  5. customdrying
  6. custom(MgSO4) and evaporation

출처 및 근거

ORD 기록
ord-f5090744201b4100aeca56b6cb08a835
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05665723

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