O-Methylhydroxylamine hydrochloride → 4-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amide

HRID 552663ノート

反応式

HRID 552663 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([N:8]=[CH:9][N:10](C)C)=[O:7])=[C:4]([CH3:15])[CH:3]=1.Cl.[CH3:17][O:18]N>O1CCOCC1.O.C(OCC)(=O)C>[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([NH:8][CH:9]=[N:10][O:18][CH3:17])=[O:7])=[C:4]([CH3:15])[CH:3]=1

参加物

6

反応物 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 666997874-Bromo-N-[(dimethylamino)methylene]-2-methylbenzamide

生成物 1

HCID 1363378164-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amide収率 103.7%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

In a solution of 0.67 g of 4-bromo-N-(dimethylaminomethylidene)-2-methyl benzoic acid amide in 10 mL of 1,4-dioxane, a solution of 0.36 g of methoxyamine hydrochloride in 2 mL of water was added, and stirred at room temperature for 1 hour. After the completion of the reaction, the reaction mixture was diluted with 50 mL of ethyl acetate, washed with water, and dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 0.70 g of the aimed product as white crystal.

後処理

  1. customAfter the completion of the reaction
  2. washwashed with water
  3. dry with materialdried over saturated sodium chloride aqueous solution
  4. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-0225d9f3e84043918ceb9419e4ad18c6
出典データセット
uspto-grants-2011_05
特許番号
US07951828B1

反応ノート

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