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Water → 2,2-Dimethyl-4-(2-methoxymethoxyphenyl)-5-oxopiperazine-1-carboxylic acid t-butyl ester

HRID 1694908
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인쇄 미리보기

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HRID 1694908 반응식
C(N(C(C)C)CC)(C)C.[CH3:10][O:11][CH2:12]Cl.[C:14]([O:18][C:19]([N:21]1[CH2:26][C:25](=[O:27])[N:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[OH:34])[CH2:23][C:22]1([CH3:36])[CH3:35])=[O:20])([CH3:17])([CH3:16])[CH3:15].O>C(Cl)Cl>[C:14]([O:18][C:19]([N:21]1[CH2:26][C:25](=[O:27])[N:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[O:34][CH2:10][O:11][CH3:12])[CH2:23][C:22]1([CH3:36])[CH3:35])=[O:20])([CH3:17])([CH3:15])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 666456104-(2-Hydroxyphenyl)-2,2-dimethyl-5-oxopiperazine-1-carboxylic acid t-butyl ester

생성물 1

HCID 666457882,2-Dimethyl-4-(2-methoxymethoxyphenyl)-5-oxopiperazine-1-carboxylic acid t-butyl ester수율 100.3%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

0.72 ml of diisopropylethylamine (4.10 mmol) and 0.16 ml of methoxymethyl chloride (2.05 mmol) were added to a solution of 400 mg of 4-(2-hydroxyphenyl)-2,2-dimethyl-5-oxopiperazine-1-carboxylic acid t-butyl ester obtained in Example (10d) (1.36 mmol) in methylene chloride (14 ml), and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction with methylene chloride. Then, the organic layer was washed with brine and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:n-hexane/ethyl acetate=1/1) to obtain 497 mg of 2,2-dimethyl-4-(2-methoxymethoxyphenyl)-5-oxopiperazine-1-carboxylic acid t-butyl ester (yield: quant.).

후처리

  1. extractionfollowed by extraction with methylene chloride
  2. washThen, the organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationAfter filtration
  5. customthe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (elution solvent:n-hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-46c989a56eed4931b8fcde1214e78e52
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158790B2

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