Pentafluoropropionic acid → HCID 178499322、化合物

HRID 2211294

反応式

HRID 2211294 の反応式
[NH2:1][C:2]1[C:6]([NH2:7])=[C:5]([CH3:8])[S:4][C:3]=1[C:9]([O:11][CH3:12])=[O:10].[F:13][C:14]([F:22])([F:21])[C:15]([F:20])([F:19])[C:16](O)=O>>[CH3:8][C:5]1[S:4][C:3]([C:9]([O:11][CH3:12])=[O:10])=[C:2]2[C:6]=1[NH:7][C:16]([C:15]([F:20])([F:19])[C:14]([F:22])([F:21])[F:13])=[N:1]2

参加物

3

反応物 2

HCID 62356Pentafluoropropionic acidHCID 18693138Methyl 3,4-diamino-5-methylthiophene-2-carboxylate

生成物 1

HCID 178499322HCID 178499322、化合物

反応条件

温度
100 °C

実験手順

A mixture of methyl 3,4-diamino-5-methylthiophene-2-carboxylate (1.0 g) in pentafluoropropionic acid (8.9 g) was stirred at 100° C. for 6 hr. The reaction solution was concentrated to dryness and the residue was suspensed in water. The mixture was made basic with aqueous solution of K2CO3, followed by extraction with ethyl acetate. The organic layer was washed with water, dried and concentrated to dryness. The residue was purified by silica gel column chromatography to give crystals. Recrystallization from isopropyl ether-hexane gave colorless plates (0.86 g, 51%). m.p. 156°-157° C.

後処理

  1. concentrationThe reaction solution was concentrated to dryness
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with water
  4. customdried
  5. concentrationconcentrated to dryness
  6. customThe residue was purified by silica gel column chromatography
  7. customto give crystals
  8. customRecrystallization from isopropyl ether-hexane
  9. customgave colorless plates (0.86 g, 51%)

出典と根拠

ORDレコード
ord-0b542faa7968475393bf06b11052ba00
出典データセット
uspto-grants-1995_10
特許番号
US05463073

関連ノート

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