Hydrochloric Acid → HCID 3053807、化合物

HRID 1578093ノート

反応式

HRID 1578093 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)=O.Cl.[C:15](=[O:18])([O-])[O-].[Na+].[Na+]>C(Cl)(Cl)Cl.O>[CH3:4][C:5]1[N:1]=[C:2]2[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]2[C:15](=[O:18])[C:6]=1[CH2:7][CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 661742-Amino-5-chloropyridine

生成物 1

HCID 3053807HCID 3053807、化合物収率 91%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

12.8 g. of 2-amino-5-chloropyridine are reacted with 15.8 g. of ethyl-2-ethylacetacetate in a mixture of 46 g. of phosphorus oxychloride and 7 g. of polyphosphoric acid at 120° to 130° C. for 3 hours. The initially violent hydrogen chloride gas evolution gradually ceases. The reaction mixture is treated with 100 ml. of water at 70° to 80° C. Upon cooling the pH-value of the mixture is adjusted to neutral with sodium carbonate. The aqueous reaction mixture is shaken with four 100-ml. portions of chloroform. The combined chloroform solutions, dried on sodium sulphate, are evaporated and ethyl acetate is distilled through the residue. 20.2 g. (91%) of 2-methyl-3-ethyl-7-chloro-4-oxo-4H-pyrido[1,2-a]pyrimidine are obtained, melting at 114° to 116° C. after recrystallization from a mixture of ethanol and ether.

後処理

  1. additionof ethyl-2-ethylacetacetate in a mixture of 46 g
  2. additionThe reaction mixture is treated with 100 ml
  3. customat 70° to 80° C
  4. temperatureUpon cooling the pH-value of the mixture
  5. dry with materialThe combined chloroform solutions, dried on sodium sulphate
  6. customare evaporated
  7. distillationethyl acetate is distilled through the residue

出典と根拠

ORDレコード
ord-1505cc9c849341d7bcc2e523cfa7d1ac
出典データセット
uspto-grants-1981_09
特許番号
US04291036

反応ノート

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