Propionate ion → Fluazifop-butyl

HRID 1648975

反応式

HRID 1648975 の反応式
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:4]=[CH:5][C:6]([O:9][C:10]2[CH:25]=[CH:24][C:13]([O:14][C:15](=[CH2:23])[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH3:22])=[O:17])=[CH:12][CH:11]=2)=[N:7][CH:8]=1.[H][H].C([O-])(=O)CC>C(O)CCC.[Pd]>[F:26][C:2]([F:1])([F:27])[C:3]1[CH:4]=[CH:5][C:6]([O:9][C:10]2[CH:25]=[CH:24][C:13]([O:14][CH:15]([CH3:23])[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH3:22])=[O:17])=[CH:12][CH:11]=2)=[N:7][CH:8]=1

参加物

6

反応物 3

HCID 104745Propionate ionHCID 20481507n-Butyl 2-[4-(5-trifluoromethylpyrid-2-yloxy)phenoxy]acrylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 50897Fluazifop-butyl

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 2631-Butanol溶媒

実験手順

The product (15 g) from Step 3 in n-butanol (300 ml) was hydrogenated at room temperature and atmospheric pressure using a 10% palladium on carbon catalyst. When the uptake of hydrogen ceased, the catalyst was filtered off and the filtrate evaporated under reduced pressure. The residue was purified by short-path distillation (at 140°-150°/0.2 mmHg) to afford a main fraction (11.6 g) containing 57% w/w of the desired propionate which was recrystallised from cold hexane to give n-butyl 2-[4-(5-trifluoromethylpyrid-2-yloxy)-phenoxy]propionate. The propionate may then be obtained substantially pure by recrystallisation from cold hexane.

後処理

  1. customwas hydrogenated at room temperature
  2. filtrationthe catalyst was filtered off
  3. customthe filtrate evaporated under reduced pressure
  4. distillationThe residue was purified by short-path distillation (at 140°-150°/0.2 mmHg)
  5. customto afford a main fraction (11.6 g)
  6. customwas recrystallised from cold hexane

出典と根拠

ORDレコード
ord-e4248a7e14cb4d4ca79cf0131ba920b0
出典データセット
uspto-grants-1983_11
特許番号
US04414391

関連ノート

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