Hydroxyamine hydrochloride → HCID 86744460、化合物

HRID 1195875ノート

反応式

HRID 1195875 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=O.Cl.[NH2:19][OH:20]>N1C=CC=CC=1>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH:12]=[N:19][OH:20]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 15027376HCID 15027376、化合物

生成物 1

HCID 86744460HCID 86744460、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-[(2,3-dimethylphenyl)amino] benzaldehyde (11 g, 0.049 mol) and hydroxylamine hydrochloride (17 g, 0.25 mol) in pyridine (250 ml) is stirred at room temperature overnight. The solvent is evaporated and the residue is partitioned between ethyl acetate (200 ml) and 10% aqueous HCl (200 ml). The organic layer is washed with 10% aqueous HCl (200 ml) and water (2×100 ml). The organic layer is dried (MgSO4) and the solvent is evaporated to give 2-[(2,3-dimethylphenyl) amino]benzaldehyde oxime which is recrystallized from hexane. Yield 7.3 g (62%); mp 107°-108° C.

後処理

  1. customThe solvent is evaporated
  2. customthe residue is partitioned between ethyl acetate (200 ml) and 10% aqueous HCl (200 ml)
  3. washThe organic layer is washed with 10% aqueous HCl (200 ml) and water (2×100 ml)
  4. dry with materialThe organic layer is dried (MgSO4)
  5. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-ed2d16ddbc8941fcb021ac0dacef2c55
出典データセット
uspto-grants-1992_05
特許番号
US05112846

反応ノート

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