FK 3311 → 4'-[1-(Tert-butyloxycarbonylmethoxyimino)ethyl]-2'-(2,4-difluorophenoxy)methanesulfonanilide

HRID 1607685노트

반응식

HRID 1607685 반응식
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[C:6]([O:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:17]=2[F:23])[CH:5]=1)(=O)[CH3:2].[NH2:24][O:25][CH2:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28]>C(O)C>[C:30]([O:29][C:27]([CH2:26][O:25][N:24]=[C:1]([C:4]1[CH:14]=[CH:13][C:7]([NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[C:6]([O:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:17]=2[F:23])[CH:5]=1)[CH3:2])=[O:28])([CH3:33])([CH3:32])[CH3:31]

참가 물질

4

반응물 2

HCID 164009FK 3311HCID 12919121tert-Butyl (aminooxy)acetate

생성물 1

HCID 543214524'-[1-(Tert-butyloxycarbonylmethoxyimino)ethyl]-2'-(2,4-difluorophenoxy)methanesulfonanilide수율 125.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4'-acetyl-2'-(2,4-difluorophenoxy)methanesulfonanilide (1.5 g) and tert-butyl aminooxyacetate (0.71 g) in ethanol (5 ml) was refluxed for 13 hours. The mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residual oil was suspended in ether and the insoluble material was filtered off. The filtrate was concentrated to give an cil of 4'-[1-(tertbutyloxycarbonylmethoxyimino)ethyl]-2'-(2,4-difluorophenoxy)methanesulfonanilide (2.6 g).

후처리

  1. temperaturewas refluxed for 13 hours
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. filtrationthe insoluble material was filtered off
  8. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-4bf3df6cc27f4952a4b45185a42c5c9a
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866091

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