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

HRID 1377525
ノート
印刷プレビュー

反応式

HRID 1377525 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f5090744201b4100aeca56b6cb08a835
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05665723

反応ノート

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