Hydrofluoric Acid → Methyl 3,5-diamino-6-fluoropyrazinoate

HRID 2083370ノート

反応式

HRID 2083370 の反応式
[NH2:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[N:4][CH:5]=[C:6]([NH2:8])[N:7]=1.[FH:13]>>[NH2:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[N:4][C:5]([F:13])=[C:6]([NH2:8])[N:7]=1

参加物

3

反応物 2

HCID 14917Hydrofluoric AcidHCID 15148126Methyl 3,5-diaminopyrazine-2-carboxylate

生成物 1

HCID 20355849Methyl 3,5-diamino-6-fluoropyrazinoate

反応条件

温度
-78 °C

実験手順

In a reactor cooled to -78° C. in an acetone-dry ice bath is placed methyl 3,5-diaminopyrazinoate (6 g.) and liquid hydrogen fluoride (70 ml.). A stream of fluorinehelium mixture (1:4 v /v) is passed through the solution for 51/2 hours at <78° C. followed by a vigorous stream of nitrogen to remove the solvent. The reaction residue is treated with conc. hydrochloric acid (60 ml.) evaporated to dryness, dissolved in water (75 ml.) and neutralized with aqueous sodium hydroxide to give methyl 3,5-diamino-6-fluoropyrazinoate (5 g.) which is purified by sublimation (140°-50° C, 0.05 mm Hg) and recrystalliation from 2-propanol.

後処理

  1. custom2 hours
  2. customat <78° C.
  3. customto remove the solvent
  4. additionThe reaction residue is treated with conc. hydrochloric acid (60 ml.)
  5. customevaporated to dryness
  6. dissolutiondissolved in water (75 ml.)

出典と根拠

ORDレコード
ord-d744c8e989d04102ad64e8f69323c892
出典データセット
uspto-grants-1978_04
特許番号
US04085211

反応ノート

読み込み中…