Dimethylformamide → 1-(3-bromopropyl)-3-methyl-2,4(1H)-quinazolinedione

HRID 247024노트

반응식

HRID 247024 반응식
[Br:1][CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[NH:7][C:6]1=[O:16].CI.[C:19](=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[Br:1][CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[N:7]([CH3:19])[C:6]1=[O:16]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 136872071-(3-bromopropyl)-2,4(1H,3H)-quinazolinedione

생성물 1

HCID 136872081-(3-bromopropyl)-3-methyl-2,4(1H)-quinazolinedione수율 62.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-(3-bromopropyl)-2,4(1H, 3H)-quinazolinedione (2.83 g), methyl iodide (3 ml), anhydrous potassium carbonate (4.2 g) and N,N-dimethylformamide (25 ml) was stirred for 8 hours at ambient temperature. After the reaction mixture was diluted with cold water, the resultant mixture was extracted twice with chloroform. The chloroform layer was washed with water twice, and with saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and evaporated in vacuo. The resultant oily residue was purified by subjecting to a column chromatography on silica gel (100 g) using chloroform for elution, to give 1-(3-bromopropyl)-3-methyl-2,4(1H)-quinazolinedione (1.85 g) as a crystal. m.p. 90°-96° C.

후처리

  1. extractionthe resultant mixture was extracted twice with chloroform
  2. washThe chloroform layer was washed with water twice
  3. dry with materialwith saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate
  4. customevaporated in vacuo
  5. customThe resultant oily residue was purified
  6. washfor elution

출처 및 근거

ORD 기록
ord-b53808ef6f6f4a34b6d25dac1e601472
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705787

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