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Ethyl Acetate → 1,1-Dimethylethyl hexahydro-4-oxo-1,1-diphenylpyrazino[2,1-c][1,4]oxazine-8(1H)-carboxylate

HRID 1713506
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HRID 1713506 반응식
Cl[CH2:2][C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH:6]1[C:18]([OH:31])([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:4].[H-].[Na+].C(OCC)(=O)C>O1CCCC1>[O:4]=[C:3]1[CH2:2][O:31][C:18]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]2[CH2:7][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:9][CH2:10][N:5]12
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 684196211,1-Dimethylethyl 4-(chloroacetyl)-3-[hydroxy(diphenyl)methyl]piperazine-1-carboxylate

생성물 1

HCID 231218541,1-Dimethylethyl hexahydro-4-oxo-1,1-diphenylpyrazino[2,1-c][1,4]oxazine-8(1H)-carboxylate수율 93.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

To a solution of 1,1-dimethylethyl 4-(chloroacetyl)-3-[hydroxy(diphenyl)methyl]piperazine-1-carboxylate (0.28 g, 0.63 mmol) in tetrahydrofuran (5 mL) was added 60% sodium hydride (40 mg, 1.0 mmol), and the mixture was stirred at room temperature for 3 hours. To the reaction solution was added ethyl acetate, and the resulting mixture was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain the title compound (0.24 g, yield 93%).

후처리

  1. washthe resulting mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b80e8206082545fab2d9f424dcad2d8e
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795267B2

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