Dimethoxymethane → T-2000

HRID 432615ノート

反応式

HRID 432615 の反応式
CO[CH2:3][O:4][CH3:5].[C:6](CS([O-])(=O)=O)(=[O:8])C.[C:14]1([C:20]2([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:25](=[O:26])[NH:24][C:23](=[O:27])[NH:22][C:21]2=[O:28])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[CH:35](N(CC)C(C)C)(C)C>CN(C)C=O.Cl.C(OCC)(=O)C>[CH3:35][O:8][CH2:6][N:22]1[C:21](=[O:28])[C:20]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[C:25](=[O:26])[N:24]([CH2:3][O:4][CH3:5])[C:23]1=[O:27]

参加物

8

反応物 4

HCID 8020DimethoxymethaneHCID 464845,5-Diphenylbarbituric acidHCID 81531DiisopropylethylamineHCID 161641Dihydroxyacetone sulfate

生成物 1

HCID 9907289T-2000

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
25 °C

実験手順

Dimethoxymethane (10.85 g) was added at 0° C. to 19.7 g of acetylmethanesulfonate. The reaction was stirred at 25° C. for 2 hours. The resultant solution was then added gradually over 45 minutes to a mixture of 10 g of 5,5-diphenylbarbituric acid and 13.85 g of N,N-diisopropyl ethyl amine in 60 ml of dry dimethylformamide. The resultant reaction mixture was stirred for about 15 minutes and then diluted with 180 ml of 2N HCl, followed by 300 ml of ethyl acetate. The phases were separated and the ethyl acetate phase was washed first with 150 ml of saturated aqueous sodium chloride and then with 150 ml of 2N aqueous NaOH. The organic (ethyl acetate) phase was dried over anhydrous sodium sulfate, filtered and concentrated to dryness to give 12.2 g of N,N′-bismethoxymethyl-5,5-diphenylbarbituric acid. Crystallization from 48 ml of toluene afforded 10.5 g of pure product (79.6% yield).

後処理

  1. customThe resultant reaction mixture
  2. stirringwas stirred for about 15 minutes
  3. customThe phases were separated
  4. washthe ethyl acetate phase was washed first with 150 ml of saturated aqueous sodium chloride
  5. dry with materialThe organic (ethyl acetate) phase was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-b421bf0075ba4a7cbfd9443c15297241
出典データセット
uspto-grants-2003_12
特許番号
US06664262B2

反応ノート

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