Ammonia → 4-Chloro-5-nitroisoquinoline

HRID 10549

反応式

HRID 10549 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[N:4][CH:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+].N>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[N+:12]([O-:14])=[O:13])[CH:5]=[N:4][CH:3]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 24434Potassium NitrateHCID 6409744-Chloroisoquinoline

生成物 1

HCID 219799674-Chloro-5-nitroisoquinoline収率 69.4%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

Intermediate 88 (375 mg) was dissolved in concentrated sulfuric acid (2 ml), then added with potassium nitrate (260 mg) with ice cooling and stirred for 2 hours. The reaction mixture was added with 28% aqueous ammonia (10 ml) and extracted twice with ethyl acetate (15 ml for each time). The organic layer was dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to obtain the title compound (332 mg).

後処理

  1. extractionextracted twice with ethyl acetate (15 ml for each time)
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-d8ae3de07dce41eb80afac012049edb2
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

関連ノート

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