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Sodium hydride → 4,6-Bis-(1,1-dimethylethyl)-5-[(2-methoxyethoxy) methoxy]-2-pyrimidine carboxylic acid methyl ester

HRID 326676
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HRID 326676 반응식
[CH3:1][O:2][C:3]([C:5]1[N:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[N:6]=1)=[O:4].[H-].[Na+].[CH3:22][O:23][CH2:24][CH2:25][O:26][CH2:27]Cl>C1COCC1.O.[NH4+].[Cl-]>[CH3:1][O:2][C:3]([C:5]1[N:6]=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:8]([O:15][CH2:22][O:23][CH2:24][CH2:25][O:26][CH3:27])=[C:9]([C:11]([CH3:12])([CH3:13])[CH3:14])[N:10]=1)=[O:4]
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참가 물질

7

반응물 3

HCID 24758Sodium hydrideHCID 775901-(Chloromethoxy)-2-methoxyethaneHCID 152753194,6-Bis (1,1-dimethylethyl)-5-hydroxy-2-pyrimidine carboxylic acid methyl ester

생성물 1

HCID 540881314,6-Bis-(1,1-dimethylethyl)-5-[(2-methoxyethoxy) methoxy]-2-pyrimidine carboxylic acid methyl ester수율 100%

시약·촉매·용매 3

HCID 962Water
용매
HCID 8028Tetrahydrofuran용매2회
HCID 25517Ammonium Chloride용매

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온도
0 °C

실험 절차

A solution of 4,6-bis-(1,1-dimethylethyl)-5-hydroxy-2-pyrimidine carboxylic acid methyl ester (4.0 g, 15.0 mmoles) in 50 mL of THF is added to a suspension of NaH (0.39 g, 16.5 mmoles) in THF (50 mL) at 0° C. When addition is complete, the reaction mixture is stirred at 0° C. for 15 minutes. 2-methoxyethoxymethyl chloride (2.0 g, 16.5 mmoles) is added and the solution is warmed to room temperature. The reaction mixture is stirred at room temperature overnight. It is diluted with 100 mL H2O and 100 mL of saturated aqueous NH4Cl. The layers are separated, and the aqueous phase is washed with Et2O (3×100 mL). The combined organic phases are washed with 100 mL brine and dried over MgSO4. Evaporation of Et2O gives 5.3 g (100%) of the desired ester as an oil.

후처리

  1. additionWhen addition
  2. temperaturethe solution is warmed to room temperature
  3. stirringThe reaction mixture is stirred at room temperature overnight
  4. customThe layers are separated
  5. washthe aqueous phase is washed with Et2O (3×100 mL)
  6. washThe combined organic phases are washed with 100 mL brine
  7. dry with materialdried over MgSO4
  8. customEvaporation of Et2O

출처 및 근거

ORD 기록
ord-3eb83e9ade39460080ea1786972bca87
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05270319

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