Isoquinoline, 1-chloro- → N-(3-Bromobenzoyl)-N-(1-isoquinolyl)hydrazine

HRID 574035

反応式

HRID 574035 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[Br:12][C:13]1[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=1)[C:16]([NH:18][NH2:19])=[O:17]>C1(C)C=CC(C)=CC=1>[Br:12][C:13]1[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=1)[C:16]([N:18]([C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1)[NH2:19])=[O:17]

参加物

4

反応物 2

HCID 140539Isoquinoline, 1-chloro-HCID 520941m-Bromobenzohydrazide

生成物 1

HCID 66709633N-(3-Bromobenzoyl)-N-(1-isoquinolyl)hydrazine収率 90.6%

試薬・触媒・溶媒 1

HCID 7809P-Xylene溶媒

反応条件

温度
150 °C

実験手順

To a 200-mL three-neck flask were added 3.3 g (20 mmol) of 1-chloroisoquinoline, 4.3 g (20 mmol) of 3-bromobenzoylhydrazine, and 80 mL of para-xylene. This mixture was refluxed at 150° C. for 14 hours under a nitrogen stream. After a predetermined time elapsed, this mixture was cooled to room temperature, and the precipitated solid was collected by suction filtration. The obtained solid was washed with toluene, a saturated aqueous solution of sodium hydrogen carbonate, and water. This solid was dried, so that the substance which was the object of the synthesis was obtained as 6.2 g of a pale yellow powder in 90% yield.

後処理

  1. temperaturethis mixture was cooled to room temperature
  2. filtrationthe precipitated solid was collected by suction filtration
  3. washThe obtained solid was washed with toluene
  4. customThis solid was dried, so that the substance which

出典と根拠

ORDレコード
ord-a111e756426347d48c5a10da0b2ef81a
出典データセット
uspto-grants-2015_05
特許番号
US09034486B2

関連ノート

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