Water → N-cyclohexyl-2,4,5-trimethylfuran-3-hydroxamic acid

HRID 1730810

反応式

HRID 1730810 の反応式
Cl.[CH:2]1([NH:8][OH:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C(=O)([O-])O.[Na+].O.[CH3:16][C:17]1[O:18][C:19]([CH3:26])=[C:20]([CH3:25])[C:21]=1[C:22](Cl)=[O:23]>ClCCl>[CH:2]1([N:8]([C:22]([C:21]2[C:20]([CH3:25])=[C:19]([CH3:26])[O:18][C:17]=2[CH3:16])=[O:23])[OH:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

6

反応物 4

HCID 962WaterHCID 516892Sodium BicarbonateHCID 3084432N-Cyclohexylhydroxylamine hydrochlorideHCID 145359342,4,5-Trimethyl-3-furancarbonyl chloride

生成物 1

HCID 21496536N-cyclohexyl-2,4,5-trimethylfuran-3-hydroxamic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

49 Parts of N-cyclohexylhydroxylamine hydrochloride is dissolved in 400 parts of dichloromethane; at room temperature a solution of 50.4 parts of sodium hydrogen carbonate in 500 parts of water and subsequently 51.6 parts of 2,4,5-trimethylfuran- 3-carboxylic chloride are added to the mixture. After the mixture has been stirred for 2 hours the dichloromethane phase is separated, dried over anhydrous sodium sulfate and evaporated. There is obtained 75 parts of N-cyclohexyl-2,4,5-trimethylfuran-3-hydroxamic acid in the form of an oil. This oil is dissolved in 300 parts of dichloromethane. To this solution there is added 36 parts of sodium hydroxide in 200 parts of water and 75.6 parts of dimethyl sulfate and the whole is stirred for 2 hours. The dichloromethane phase is then separated, washed with water until neutral, dried over anhydrous sodium sulfate and evaporated. Upon distillation of the residue there is obtained 52 parts of O-methyl-N-cyclohexyl-2,4,5-trimethylfuran-3-hydroxamic acid having a boiling point at 0.3 mm Hg of 128° to 130° C and the refractive index nD25 : 1.5021. ##SPC11##

後処理

  1. customis separated
  2. dry with materialdried over anhydrous sodium sulfate
  3. customevaporated

出典と根拠

ORDレコード
ord-69d4ab0d52e04d5394e67c84a103ebd5
出典データセット
uspto-grants-1976_11
特許番号
US03993772

関連ノート

読み込み中…