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Dimethylamine → HCID 85945614, 화합물

HRID 1455008
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HRID 1455008 반응식
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9](Cl)=[O:10])=[C:4]([Cl:12])[N:3]=1.C(=O)(O)[O-].[Na+].[CH3:18][NH:19][CH3:20]>C(Cl)Cl.O>[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]([N:19]([CH3:20])[CH3:18])=[O:10])=[C:4]([Cl:12])[N:3]=1
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참가 물질

6

반응물 3

HCID 674DimethylamineHCID 516892Sodium BicarbonateHCID 132643612,4,6-Trichloropyrimidine-5-carbonyl chloride

생성물 1

HCID 85945614HCID 85945614, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of the subtitle product of step ii) (2.0 g) in DCM (20 ml) and sodium bicarbonate (1.36 g) in water (20 ml) at 0° C. was added dimethylamine (1.00 ml, 40% aqueous) dropwise. The reaction mixture was stirred at room temperature for 2 h before DCM (40 ml) was added and the aqueous layer separated. The organic layer was washed with water (20 ml), brine (10 ml) and dried (MgSO4). The solid was filtered and the solvent evaporated to dryness under reduced pressure. The residue was purified by column chromatography (EtOAc/isohexane (1:1)) to yield the subtitle compound as an off white solid. Yield 1.9 g

후처리

  1. additionwas added
  2. customthe aqueous layer separated
  3. washThe organic layer was washed with water (20 ml), brine (10 ml)
  4. dry with materialdried (MgSO4)
  5. filtrationThe solid was filtered
  6. customthe solvent evaporated to dryness under reduced pressure
  7. customThe residue was purified by column chromatography (EtOAc/isohexane (1:1))

출처 및 근거

ORD 기록
ord-06b5000d3d9843c4bcd11a028cee8356
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482355B2

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