Homoallyl bromide → HCID 13298148, 화합물

HRID 1706369

반응식

HRID 1706369 반응식
Br[CH2:2][CH2:3][CH:4]=[CH2:5].[N:6]1([C:17](=[O:18])[C:16]2[NH:15][CH:14]=[N:13][C:12]=2[N:10]([CH3:11])[C:8]1=[O:9])[CH3:7].[Na]>CN(C)C=O>[CH3:7][N:6]1[C:17](=[O:18])[C:16]2[N:15]([CH2:2][CH2:3][CH:4]=[CH2:5])[CH:14]=[N:13][C:12]=2[N:10]([CH3:11])[C:8]1=[O:9]

참가 물질

4

반응물 2

HCID 21241Homoallyl bromideHCID 669736033,7-Dihydro-1,3-dimethyl-1H-purine-2,6-dione, sodium salt

생성물 1

HCID 13298148HCID 13298148, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

13.9 g of 4-bromo-but-1-ene are reacted with 20.2 g of sodium theophylline in 200 ml of dimethyl-formamide at 120° C. with stirring for approximately 6 to 8 hours until the reaction is complete as indicated by thin-layer chromatography. The solvent is then removed under reduced pressure. The residue is dissolved at 20° C. in 100 ml of methylene chloride, separated from insoluble sodium bromide and purified through a column packed with neutral aluminum oxide to remove small quantities of dark-coloured accompanying substances. Melting point: 110° C. (acetone); yield: 21.6 g (91% of theory relative to the starting material used). After thin-layer chromatography on Merck DC finished plates of silica gel 60 F254 with benzene/acetone (6:4) as eluent, the product has an Rf value of 0.54; and with nitromethane/benzene/pyridine (20:10:3) as eluent, an Rf value of 0.65. Utra-violet light was used as indicator, the pyridine of the eluent having, however, to be removed at 50° C. under reduced pressure because of its property to extinguish fluorescence.

후처리

  1. customThe solvent is then removed under reduced pressure
  2. dissolutionThe residue is dissolved at 20° C. in 100 ml of methylene chloride
  3. customseparated from insoluble sodium bromide
  4. custompurified through a column
  5. customto remove small quantities of dark-coloured accompanying substances
  6. customhowever, to be removed at 50° C. under reduced pressure because of its property

출처 및 근거

ORD 기록
ord-5a5b1dcd0f4a429480a540dbf9f63359
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04207321

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