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Dimethoxymethane → T-2000

HRID 1610777
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HRID 1610777 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

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

생성물 1

HCID 9907289T-2000

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

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 2 N 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. Crystalization from 48 ml of toluene afforded 10.5 g of pure product (79.6% yield).

후처리

  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

출처 및 근거

ORD 기록
ord-55d9744236b840418d66022a271c1470
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE038934E1

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