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Sodium ethoxide → 5-Methylpyrimidine-4,6-diol

HRID 2358206
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HRID 2358206 반응식
CC[O-].[Na+].Cl.[CH:6]([NH2:8])=[NH:7].C[CH2:10][CH:11]([C:16](OCC)=[O:17])[C:12](OC)=[O:13]>C(O)C>[OH:13][C:12]1[C:11]([CH3:10])=[C:16]([OH:17])[N:8]=[CH:6][N:7]=1
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참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 5088009HCID 5088009, 화합물HCID 10313058Methanimidamide, hydrochloride (1:1)

생성물 1

HCID 1784317855-Methylpyrimidine-4,6-diol수율 60%

시약·촉매·용매 1

HCID 702Ethanol용매3회

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온도
0 °C

실험 절차

102 ml (282 mmoles) of a solution of sodium ethylate at 21% in ethanol is added to a solution of 7.5 g (94 mmoles) of formamidine hydrochloride in 250 ml of ethanol cooled down to 0° C. and the mixture is stirred for 30 minutes; then a solution of 13 ml (94 mmoles) of diethyl methyl malonate in 50 ml of ethanol is added followed by stirring overnight at ambient temperature. The reaction mixture is evaporated to dryness under reduced pressure (2 kPa) and the residue is taken up in ethyl acetate, water and acetic acid in order to adjust the pH to 6. The precipitate is filtered then washed successively with water, isopropanol, diethyl ether and finally with pentane. 7 g (Yield=60%) of expected product is obtained in the form of a beige solid.

후처리

  1. stirringby stirring overnight at ambient temperature
  2. customThe reaction mixture is evaporated to dryness under reduced pressure (2 kPa)
  3. filtrationThe precipitate is filtered
  4. washthen washed successively with water, isopropanol, diethyl ether and finally with pentane

출처 및 근거

ORD 기록
ord-74d6eb1cbb9e47d1af59743564944b90
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763621B2

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