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

HRID 1607685ノート

反応式

HRID 1607685 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4bf3df6cc27f4952a4b45185a42c5c9a
出典データセット
uspto-grants-1989_09
特許番号
US04866091

反応ノート

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