Naphthalic anhydride, 3-nitro- → 2-Hydroxy-5-(hydroxy(oxido)amino)-1H-benzo(de)isoquinoline-1,3(2H)-dione

HRID 566998ノート

反応式

HRID 566998 の反応式
Cl.[NH2:2][OH:3].[CH:4]1[CH:13]=[C:12]2[C:14]([O:16][C:17](=O)[C:10]3=[C:11]2[C:6](=[CH:7][C:8]([N+:19]([O-:21])=[O:20])=[CH:9]3)[CH:5]=1)=[O:15]>N1C=CC=CC=1.O>[OH:3][N:2]1[C:17](=[O:16])[C:10]2[CH:9]=[C:8]([N+:19]([O-:21])=[O:20])[CH:7]=[C:6]3[C:11]=2[C:12](=[CH:13][CH:4]=[CH:5]3)[C:14]1=[O:15]

参加物

5

反応物 2

HCID 18194Naphthalic anhydride, 3-nitro-HCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 2721422-Hydroxy-5-(hydroxy(oxido)amino)-1H-benzo(de)isoquinoline-1,3(2H)-dione収率 99.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒

実験手順

Hydroxylamine hydrochloride (0.9 g, 13.0 mmol) was added to a suspension of 3-nitro-1,8-naphthalic anhydride (2.0 g, 8.2 mmol) in pyridine (30 mL). The mixture was refluxed for 3 hours and concentrated in vacuo to give a brown solid. The solid was suspended in water, stirred, filtered, and dried to give 2.1 g of the title compound, mp 277-279° C.

後処理

  1. temperatureThe mixture was refluxed for 3 hours
  2. concentrationconcentrated in vacuo
  3. customto give a brown solid
  4. filtrationfiltered
  5. customdried

出典と根拠

ORDレコード
ord-bad38973c14c4835b99ffdc05d2825ba
出典データセット
uspto-grants-2001_01
特許番号
US06177423B1

反応ノート

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