Hydroxyamine hydrochloride → 4-methoxy-2,3-dihydro-1H-inden-1-one oxime

HRID 384973

反応式

HRID 384973 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][C:7]2=O.[NH2:13][OH:14].Cl.C([O-])(=O)C.[Na+]>CO>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:4]=1[CH2:5][CH2:6][C:7]2=[N:13][OH:14]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 45474914-methoxy-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 766564544-methoxy-2,3-dihydro-1H-inden-1-one oxime収率 99%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4-methoxy-2,3-dihydro-1H-inden-1-one (1.0 g, 1.0 eq.) in 25 ml MeOH was added NH2OH.HCl (0.493 g, 1.15 eq.) and sodium acetate (0.597 g, 1.18 eq.). The resulting mixture was stirred at room temperature overnight. The reaction mixture was diluted with 100 ml ice-water. The white precipitate was collected by filtration, washed with 3×20 ml water and dried in vacuo to afford 1.08 g (yield 99%) 4-methoxy-2,3-dihydro-1H-inden-1-one oxime which was used to next step without further purification.

後処理

  1. filtrationThe white precipitate was collected by filtration
  2. washwashed with 3×20 ml water
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-d3a87c1c72994cb09db54a91dd7ee20b
出典データセット
uspto-grants-2013_02
特許番号
US08367836B2

関連ノート

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