Ethyl bromoacetate → Ethyl 3,6-dihydro-3-(methoxymethyl)-5-nitro-2,6-dioxo-1(2H)-pyrimidineacetate

HRID 849293

반응식

HRID 849293 반응식
[N+:1]([C:4]1[C:5](=[O:14])[NH:6][C:7](=[O:13])[N:8]([CH2:10][O:11][CH3:12])[CH:9]=1)([O-:3])=[O:2].Br[CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18]>[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1>[N+:1]([C:4]1[C:5](=[O:14])[N:6]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:7](=[O:13])[N:8]([CH2:10][O:11][CH3:12])[CH:9]=1)([O-:3])=[O:2]

참가 물질

5

반응물 2

HCID 7748Ethyl bromoacetateHCID 181724885-Nitro-1-methoxymethyluracil

생성물 1

HCID 21355699Ethyl 3,6-dihydro-3-(methoxymethyl)-5-nitro-2,6-dioxo-1(2H)-pyrimidineacetate

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 2724141Tetrabutylammonium Fluoride용매

실험 절차

The compound of Example 41 (10.0 g, 50 mmole) is dissolved in tetrabutylammonium flouride (120 mL of a 1.0M solution in tetrahydrofuran, 0.124 mole). Ethyl bromoacetate (8.3 mL, 75 mmole) is added. The reaction mixture is stirred at room temperature. The reaction mixture is concentrated, then partitioned between dichloromethane and water. The aqueous layer is extracted with dichloromethane. The combined organic extracts are washed with water, brine, and dried over anhydrous magnesium sulfate. The solvent is removed under vacuum to afford the title compound.

후처리

  1. concentrationThe reaction mixture is concentrated
  2. custompartitioned between dichloromethane and water
  3. extractionThe aqueous layer is extracted with dichloromethane
  4. washThe combined organic extracts are washed with water, brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent is removed under vacuum

출처 및 근거

ORD 기록
ord-eb15bb1238e34312a75af867177ad000
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06011158

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