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Carbamimidic acid, methyl ester, sulfate (1:1) → HCID 178494253, 화합물

HRID 2261164
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HRID 2261164 반응식
CC[O-].[Na+].S(O)(O)(=O)=O.[CH3:10][O:11][C:12]([NH2:14])=[NH:13].C[CH2:16][CH:17]([C:22](OCC)=[O:23])[C:18](OC)=[O:19]>C(O)C>[CH3:10][O:11][C:12]1[N:14]=[C:18]([OH:19])[C:17]([CH3:16])=[C:22]([OH:23])[N:13]=1
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참가 물질

5

반응물 3

HCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)HCID 2723922Sodium ethoxideHCID 5088009HCID 5088009, 화합물

생성물 1

HCID 178494253HCID 178494253, 화합물수율 72.7%

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
0 °C

실험 절차

13.8 g (200 mmoles) of sodium ethylate is added to a solution of 10 g (58 mmoles) of methoxyformamidine sulphate in 100 ml of ethanol cooled down to 0° C. and the mixture is stirred for 15 minutes; then a solution of 9 ml (52 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). The residue is taken up in 100 ml of a saturated solution of sodium chloride and extracted with 800 and 200 ml of n-butanol. The organic phases are dried over sodium sulphate, filtered and evaporated to dryness under reduced pressure (2 kPa). 5.9 g of expected product is obtained in the form of a white solid.

후처리

  1. stirringby stirring overnight at ambient temperature
  2. customThe reaction mixture is evaporated to dryness under reduced pressure (2 kPa)
  3. extractionextracted with 800 and 200 ml of n-butanol
  4. dry with materialThe organic phases are dried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure (2 kPa)

출처 및 근거

ORD 기록
ord-1a4f81d05f6a47ec9d61945f013dc676
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07846932B2

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