Ethanol → (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)-methylaminocarbonylmethylpyridinium chloride

HRID 2232205

反応式

HRID 2232205 の反応式
[Cl:1][CH2:2][C:3]([NH:5][CH2:6][C:7]1[C:15]([OH:16])=[C:14]2[C:10]([CH2:11][CH2:12][C:13]2=O)=[C:9]([CH3:18])[CH:8]=1)=O.Cl.[NH2:20][OH:21].[N:22]1[CH:27]=[CH:26]C=C[CH:23]=1.[CH2:28](O)[CH3:29].[OH2:31]>>[Cl-:1].[OH:16][C:15]1[C:7]([C:6]2[CH:29]=[CH:28][CH:2]=[CH:3][N+:5]=2[CH2:26][C:27]([NH:22][CH3:23])=[O:31])=[CH:8][C:9]([CH3:18])=[C:10]2[C:14]=1[C:13](=[N:20][OH:21])[CH2:12][CH2:11]2

参加物

6

反応物 5

HCID 702EthanolHCID 962WaterHCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 136041414-Methyl-6-alpha-chloroacetylaminomethyl-7-hydroxy-1-indanone

生成物 1

HCID 136342833(2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)-methylaminocarbonylmethylpyridinium chloride

実験手順

200 Grams of 6-chloroacetylaminomethyl-2,3-dihydro-7-hydroxy-4-methyl-1H-indene-1-one, 77.9 g of hydroxylamine hydrochloride, 300 ml of pyridine and 1,800 ml of ethanol were refluxed for 3 hours. After the reaction was completed, the solvent was removed by evaporation under a reduced pressure, then to the residue thus obtained was added 2 liters of water and the mixture was stirred vigorously, cooled and crystallized. The crystals were collected by filtration, washed with water, and recrystallized from water to obtain 167 g of (2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)-methylaminocarbonylmethylpyridinium chloride. Colorless flake-like crystals. Melting point: 279° C. (Decomposed).

後処理

  1. customthe solvent was removed by evaporation under a reduced pressure
  2. customto the residue thus obtained
  3. temperaturecooled
  4. customcrystallized
  5. filtrationThe crystals were collected by filtration
  6. washwashed with water
  7. customrecrystallized from water

出典と根拠

ORDレコード
ord-9da84f27b5424d6c987c0a1b819968f2
出典データセット
uspto-grants-1988_11
特許番号
US04788130

関連ノート

読み込み中…