Bromine → 4-Bromo-2-(2,2,2-trichloroethoxycarbonylmethoxyimino)-3-oxobutyric acid

HRID 1088107ノート

反応式

HRID 1088107 の反応式
[Cl:1][C:2]([Cl:22])([Cl:21])[CH2:3][O:4][C:5]([CH2:7][O:8][N:9]=[C:10]([C:18](=[O:20])[CH3:19])[C:11]([O:13]C(C)(C)C)=[O:12])=[O:6].[Br:23]Br>C(O)(=O)C>[Br:23][CH2:19][C:18](=[O:20])[C:10](=[N:9][O:8][CH2:7][C:5]([O:4][CH2:3][C:2]([Cl:22])([Cl:21])[Cl:1])=[O:6])[C:11]([OH:13])=[O:12]

参加物

4

反応物 2

HCID 24408BromineHCID 53973099Tert-butyl 2-(2,2,2-trichloroethoxycarbonylmethoxyimino)-3-oxobutyrate

生成物 1

HCID 538664824-Bromo-2-(2,2,2-trichloroethoxycarbonylmethoxyimino)-3-oxobutyric acid収率 98.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of tert-butyl 2-(2,2,2-trichloroethoxycarbonylmethoxyimino)-3-oxobutyrate (29.5 g) in acetic acid (59 ml) was added bromine (23.2 g) at 52° C., and the mixture was stirred at 52° to 68° C. for 15 minutes. After removal of the acetic acid from the reaction mixture under reduced pressure, the residual oil was dissolved in ethyl acetate (400 ml). The solution was washed with 10% hydrochloric acid (20 ml) and a saturated aqueous sodium chloride, followed by drying over magnesium sulfate. Removal of the solvent gave 4-bromo-2-(2,2,2-trichloroethoxycarbonylmethoxyimino)-3-oxobutyric acid (30.7 g).

後処理

  1. customAfter removal of the acetic acid from the reaction mixture under reduced pressure
  2. dissolutionthe residual oil was dissolved in ethyl acetate (400 ml)
  3. washThe solution was washed with 10% hydrochloric acid (20 ml)
  4. dry with materialby drying over magnesium sulfate
  5. customRemoval of the solvent

出典と根拠

ORDレコード
ord-1522ae61d8f1404a9362737282b729d5
出典データセット
uspto-grants-1990_10
特許番号
US04960889

反応ノート

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