Acetic Acid → HCID 178493933, 화합물

HRID 729751

반응식

HRID 729751 반응식
Cl.[CH:2]([NH2:4])=[NH:3].CC[O-].[Na+].[CH3:9][O:10][CH:11]([C:16](OC)=[O:17])[C:12](OC)=[O:13].C(O)(=O)C>C(O)C>[CH3:9][O:10][C:11]1[C:12]([OH:13])=[N:3][CH:2]=[N:4][C:16]=1[OH:17]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 78718Dimethyl methoxymalonateHCID 2723922Sodium ethoxideHCID 10313058Methanimidamide, hydrochloride (1:1)

생성물 1

HCID 178493933HCID 178493933, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

5 g (6.2 mmoles) of formamidine hydrochloride is added at 0° C. and in small quantities into a single-necked flask containing 30 ml of absolute ethanol and 90 ml of a solution of sodium ethylate at a concentration of 1.7 mol/l in ethanol. Stirring is maintained at ambient temperature for about twenty minutes, then 8.5 ml of dimethyl methoxymalonate is added dropwise. Stirring is maintained for 16 hours. The reaction mixture is then acidified with pure acetic acid to a pH between 4 and 5, then concentrated to dryness in the presence of cyclohexane. After impasting the crude product obtained is chromatographed on silicagel eluting with a mixture of methylene chloride-methanol (85-15)and 2% water-acetic acid (1-1). 9.5 g of the expected product is obtained containing a small quantity of sodium acetate salts.

후처리

  1. stirringStirring
  2. temperatureis maintained for 16 hours
  3. concentrationconcentrated to dryness in the presence of cyclohexane
  4. customobtained
  5. customis chromatographed
  6. washon silicagel eluting with a mixture of methylene chloride-methanol (85-15)and 2% water-acetic acid (1-1)

출처 및 근거

ORD 기록
ord-c196fe37c24c46fa8843bc802cc48135
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582640B2

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