Potassium Carbonate → 1-Benzyl-3-(hydroxyimino)-4-methylpyrrolidine

HRID 358908ノート

反応式

HRID 358908 の反応式
[CH2:1]([N:8]1[CH2:12][CH:11]([CH3:13])[C:10](=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:16][OH:17].C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[CH2:1]([N:8]1[CH2:12][CH:11]([CH3:13])[C:10](=[N:16][OH:17])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 124309801-Benzyl-4-methylpyrrolidin-3-one

生成物 1

HCID 859932571-Benzyl-3-(hydroxyimino)-4-methylpyrrolidine収率 107.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A solution of 31.7 g (0.168 mole) of 1-benzyl-4-methyl-3-pyrrolidone [prepared as described in Step (4) above] dissolved in 200 ml of ethanol was added dropwise to a solution of 59.4 g (0.79 mole) of hydroxylamine hydrochloride dissolved in 200 ml of water over a period of 1 hour, whilst keeping the temperature at 20° to 25° C. 62.1 g (0.45 mole) of potassium carbonate were then added, and the mixture was stirred at room temperature overnight, after which it was diluted with 100 ml of water. The aqueous solution was extracted with chloroform, and the chloroform extract was washed with water, dried and concentrated by evaporation under reduced pressure, to give 36.9 g of 1-benzyl-3-(hydroxyimino)-4-methylpyrrolidine as brown crystals.

後処理

  1. customat 20° to 25° C
  2. extractionThe aqueous solution was extracted with chloroform
  3. extractionthe chloroform extract
  4. washwas washed with water
  5. customdried
  6. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-fac065dec23f4efab27fae3f72637d10
出典データセット
uspto-grants-1991_03
特許番号
US04997943

反応ノート

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