Methyl iodide → HCID 4028144, 화합물

HRID 568338노트

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HRID 568338 반응식
[CH3:1][C:2]1[NH:7][C:6](=[S:8])[NH:5][CH:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19].[C:23](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O.C(OCC)(=O)C>[CH3:1][C:2]1[NH:7][C:6]([S:8][CH3:23])=[N:5][CH:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[C:3]=1[C:18]([O:20][CH2:21][CH3:22])=[O:19]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 2787683ethyl 6-methyl-4-(3-nitrophenyl)-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate

생성물 1

HCID 4028144HCID 4028144, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 1,2,3,4-tetrahydro-6-methyl-4-(3-nitrophenyl)-2-thioxo-5-pyrimidinecarboxylic acid, ethyl ester (1.0 g., 3.1 mmole) in dry acetone (10 ml.) is treated with finely ground potassium carbonate (1.0 g.) and methyl iodide (220 μl., 3.5 mmole). The reaction flask is tightly stoppered and the suspension is allowed to stir at room temperature overnight. It is then diluted with ethyl acetate and the white solid is filtered off. The filtrate is washed with water and brine. After drying over anhydrous magnesium sulfate, the solvent is stripped off to give a light yellow foam. Crystallization from etherhexane provides 820 mg. of off-white crystalline product. This material is combined with that from another run (200 mg.) and triturated with hexane to give an analytically pure sample of 1,4-dihydro-6-methyl-2-(methylthio)-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, ethyl ester; m.p. 91.5°-93°. TLC (silica gel; ethyl acetate: hexane, 40:60) Rf =0.36.

후처리

  1. filtrationthe white solid is filtered off
  2. washThe filtrate is washed with water and brine
  3. dry with materialAfter drying over anhydrous magnesium sulfate
  4. customto give a light yellow foam
  5. customCrystallization from etherhexane
  6. customprovides 820 mg
  7. customtriturated with hexane

출처 및 근거

ORD 기록
ord-372af9f2f9e64c33bb6282a169f18909
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728652

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