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Water → HCID 58994170、化合物

HRID 12654
ノート
印刷プレビュー

反応式

HRID 12654 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 58994170HCID 58994170、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1a75229b12604ed7ac0796073c57a14f
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07727988B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート