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

HRID 247024ノート

反応式

HRID 247024 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b53808ef6f6f4a34b6d25dac1e601472
出典データセット
uspto-grants-1987_11
特許番号
US04705787

反応ノート

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