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Methyl iodide → HCID 178503546, 화합물

HRID 1094491
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HRID 1094491 반응식
[O:1]=[C:2]1[NH:7][C:6](=[S:8])[NH:5][C:4]([CH2:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16]([C:20]([OH:22])=[O:21])=[CH:15][CH:14]=[CH:13]3)=[CH:3]1.[OH-].[Na+].[CH3:25]I>C1COCC1.O>[OH:1][C:2]1[N:7]=[C:6]([S:8][CH3:25])[N:5]=[C:4]([CH2:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[C:16]([C:20]([OH:22])=[O:21])=[CH:15][CH:14]=[CH:13]3)[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 866651666-(6-Oxo-2-thioxo-1,2,3,6-tetrahydro-pyrimidin-4-ylmethyl)-naphthalene-1-carboxylic acid

생성물 1

HCID 178503546HCID 178503546, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

2.30 g (7.37 mMol) 6-(6-oxo-2-thioxo-1,2,3,6-tetrahydro-pyrimidin-4-ylmethyl)-naphthalene-1-carboxylic acid are suspended in 160 ml THF. Then a solution of 452 mg (11.3 mMol) NaOH in 9 ml water is added, followed by 556 μl (8.93 mMol) methyliodide. After 15 h, the reaction mixture is concentrated in vacuo. The residue is used without further purification in Step 3.8. Pure title compound can be obtained by chromatography (Combi Flash; CH2Cl2→CH2Cl2/MeOH 7:1): TLC (CH2Cl2/MeOH 4:1): Rf=0.46.

후처리

  1. concentrationthe reaction mixture is concentrated in vacuo
  2. customThe residue is used without further purification in Step 3.8

출처 및 근거

ORD 기록
ord-c835a81748c94977b13618ea2369af57
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08133886B2

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