Propionate ion → Fluazifop-butyl

HRID 1648975

반응식

HRID 1648975 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 50897Fluazifop-butyl

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 2631-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e4248a7e14cb4d4ca79cf0131ba920b0
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414391

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