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

HRID 345137노트

반응식

HRID 345137 반응식
[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:4].Cl.[NH2:20][OH:21].[N:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(O)C>O>[Cl-:1].[OH:16][C:15]1[C:7]([CH2:6][NH:5][C:3]([CH2:2][N+:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:4])=[CH:8][C:9]([CH3:18])=[C:10]2[C:14]=1[C:13](=[N:20][OH:21])[CH2:12][CH2:11]2

참가 물질

6

반응물 4

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

생성물 1

HCID 136364579(2,3-dihydro-7-hydroxy-1-hydroxyimino-4-methyl-1H-indene-6-yl)methylaminocarbonylmethylpyridinium chloride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c0707d3ccdc843fe973022c3f7b11928
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055474

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