Acetic Acid → HCID 178493933、化合物

HRID 729751

反応式

HRID 729751 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 178493933HCID 178493933、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c196fe37c24c46fa8843bc802cc48135
出典データセット
uspto-grants-2009_09
特許番号
US07582640B2

関連ノート

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