Formic Acid → HCID 23453298、化合物

HRID 1277722ノート

反応式

HRID 1277722 の反応式
[NH:1]([C:3]1[CH:4]=[CH:5][C:6]([O:14][CH3:15])=[C:7]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:8]=1)[NH2:2].[CH:16]([O-])=[O:17].[Na+].C(O)=O>C(O)C>[CH:16]([NH:2][NH:1][C:3]1[CH:4]=[CH:5][C:6]([O:14][CH3:15])=[C:7]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:8]=1)=[O:17]

参加物

5

反応物 3

HCID 284Formic AcidHCID 2723810Sodium FormateHCID 234533053-(5-Hydrazino-2-methoxyphenyl)propionic acid

生成物 1

HCID 23453298HCID 23453298、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-(5-Amino-2-methoxyphenyl)propionic acid (4 g, 0.02 mole), concentrated hydrochloric acid (30 ml) and water (45 ml) were stirred together at 0°. The mixture was treated with sodium nitrite (1.38 g, 0.02 mole) in water (10 ml) at 0°. The solution was then stirred for a further one-half hour. The excess of nitrous acid was destroyed with urea. The above reaction mixture was added to a solution of stannous chloride (7.6 g) in concentrated hydrochloric acid (10 ml). The precipitate (5 g) was collected by filtration. Free hydrazine was obtained from a concentrated aqueous solution of the crude hydrochloride by addition of saturated aqueous solution of sodium acetate. A mixture of 3-(5-hydrazino-2-methoxyphenyl)propionic acid (8.8 g, 0.025 mole), sodium formate (2.8 g, 0.04 mole), formic acid (18 ml) and ethanol (60 ml) was heated under reflux for one hour. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate (1 liter). The organic layer was then washed with water and dilute aqueous hydrochloric acid (1 percent). The organic layer was dried with sodium sulphate, the solvent was removed under reduced pressure and the residue crystallized from water (5 g).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for one hour
  3. customThe solvents were removed under vacuum
  4. dissolutionthe residue was dissolved in ethyl acetate (1 liter)
  5. washThe organic layer was then washed with water and dilute aqueous hydrochloric acid (1 percent)
  6. dry with materialThe organic layer was dried with sodium sulphate
  7. customthe solvent was removed under reduced pressure
  8. customthe residue crystallized from water (5 g)

出典と根拠

ORDレコード
ord-4746caa36223432dbc4bbd9dc131e59a
出典データセット
uspto-grants-1981_07
特許番号
US04278748

反応ノート

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