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Water → [2-(4-Methoxy-5-nitro-pyrimidin-2-yloxy)-ethyl]-propyl-carbamic acid tert-butyl ester

HRID 390293
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HRID 390293 반응식
[C:1]([O:5][C:6](=[O:14])[N:7]([CH2:11][CH2:12][OH:13])[CH2:8][CH2:9][CH3:10])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].Cl[C:18]1[N:23]=[C:22]([O:24][CH3:25])[C:21]([N+:26]([O-:28])=[O:27])=[CH:20][N:19]=1.O>C1COCC1>[C:1]([O:5][C:6](=[O:14])[N:7]([CH2:11][CH2:12][O:13][C:18]1[N:23]=[C:22]([O:24][CH3:25])[C:21]([N+:26]([O-:28])=[O:27])=[CH:20][N:19]=1)[CH2:8][CH2:9][CH3:10])([CH3:2])([CH3:3])[CH3:4]
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참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 38016162-Chloro-4-methoxy-5-nitropyrimidineHCID 14925143(2-Hydroxy-ethyl)-propyl-carbamic acid tert-butyl ester

생성물 1

HCID 66882150[2-(4-Methoxy-5-nitro-pyrimidin-2-yloxy)-ethyl]-propyl-carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To a solution of (2-hydroxy-ethyl)-propyl-carbamic acid tert-butyl ester (1.07 g, 5.28 mmol) in THF (40 ml) at 0° C. was added NaH (0.25 g, 5.80 mmol). After stirring the suspension at 0° C. for 30 minutes a solution of 2-chloro-4-methoxy-5-nitropyrimidine (1 g, 5.28 mmol) in THF (10 ml) was added and the mixture was stirred at room temperature for 16 h. The mixture was added to water, which was extracted three times with dichloromethane. The combined organic layers were dried over MgSO4, filtered and concentrated under reduced pressure to obtain the title compound.

후처리

  1. additionwas added
  2. extractionwas extracted three times with dichloromethane
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-655a99571ab9415eb30d5c8a6b6fe233
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383641B2

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