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Water → HCID 58994170, 화합물

HRID 12654
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HRID 12654 반응식
[N:1]1([C:6]2[C:7](=[O:13])[NH:8][C:9](=[O:12])[NH:10][CH:11]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Br[CH2:21][CH2:22][CH2:23][Cl:24].O>CN(C=O)C>[Cl:24][CH2:23][CH2:22][CH2:21][N:10]1[CH:11]=[C:6]([N:1]2[CH2:2][CH2:3][CH2:4][CH2:5]2)[C:7](=[O:13])[NH:8][C:9]1=[O:12]
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참가 물질

6

반응물 4

HCID 962WaterHCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 172750485-(pyrrolidin-1-yl)pyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 58994170HCID 58994170, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 5-(1-pyrrolidinyl)-2,4(1H,3H)-pyrimidinedione (507 mg, commercially available from Interchim Intermediates) and K2CO3 (386 mg) in dry DMF (10 mL) was stirred for 1 hour at room temperature. 1-Bromo-3-chloropropane (0.28 mL) was added and the mixture was stirred at room temperature for 20 hours. Water was added and the resulting mixture was extracted with ethyl acetate. The organic phases were washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by a silica flash chromatography (eluting with A: dichloromethane, B: dichloromethane/methanol=9/1 at ratio A:B=6:4) to give the title compound as a colourless oil (150 mg).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe organic phases were washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by a silica flash chromatography (
  6. washeluting with A: dichloromethane, B

출처 및 근거

ORD 기록
ord-1a75229b12604ed7ac0796073c57a14f
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07727988B2

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