76700-85-1 → HCID 20202839、化合物

HRID 544577ノート

反応式

HRID 544577 の反応式
[F:1][C:2]([F:12])([F:11])[CH2:3][NH:4][C:5]([NH:7][C:8]([NH2:10])=[S:9])=[NH:6].Cl[CH2:14][C:15](=O)[CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20]>CCO>[F:12][C:2]([F:1])([F:11])[CH2:3][N:4]=[C:5]([NH2:6])[NH:7][C:8]1[S:9][CH:14]=[C:15]([CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[N:10]=1

参加物

4

反応物 2

HCID 1111662576700-85-1HCID 178512206HCID 178512206、化合物

生成物 1

HCID 20202839HCID 20202839、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To 2,2,2-trifluoroethylamidinothiourea (2.1 g.) in hot EtOH (20 ml.) was added a solution of methyl 6-chloro-5-oxohexanoate (2.0 g.) in hot EtOH (20 ml.). The mixture was heated under reflux for 1 hour and then evaporated to dryness. The residue was partitioned between ether (20 ml.) and water (60 ml.). The aqueous layer was separated, basified with sodium bicarbonate and extracted with EtOAc. The organic layer was evaporated to dryness to give a gum which was recrystallised from EtOAc/ether/acetone to give methyl 4-[2-(2-[2,2,2-trifluoroethyl]guanidino)thiazol-4-yl]butyrate which was used without further purification.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. customevaporated to dryness
  4. customThe residue was partitioned between ether (20 ml.) and water (60 ml.)
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc
  7. customThe organic layer was evaporated to dryness
  8. customto give a gum which
  9. customwas recrystallised from EtOAc/ether/acetone

出典と根拠

ORDレコード
ord-b6e9ce6f7c9249bcac5b934657157ae6
出典データセット
uspto-grants-1984_05
特許番号
US04451463

反応ノート

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