Water → HCID 59620340、化合物

HRID 1887744ノート

反応式

HRID 1887744 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([N+:12]([O-])=O)[CH:11]=1)[NH:8][C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:19])[CH3:18])[CH2:5]2.C([O-])=O.[NH4+].O>C(O)C.[Pd]>[NH2:12][C:10]1[CH:11]=[CH:2][CH:3]=[C:4]2[C:9]=1[NH:8][C:7](=[O:15])[CH:6]([NH:16][C:17](=[O:19])[CH3:18])[CH2:5]2

参加物

6

反応物 3

HCID 962WaterHCID 2723923Ammonium formateHCID 59620398HCID 59620398、化合物

生成物 1

HCID 59620340HCID 59620340、化合物収率 84.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒2 回

反応条件

温度
80 °C

実験手順

N-(6-Bromo-8-nitro-2-oxo-1,2,3,4-tetrahydroquinolin-3-yl)acetamide (15 g) was suspended in ethanol (150 mL), and ammonium formate (28.8 g) and 10% Pd—C (water content: 53%) (1.5 g) were added thereto. The mixture was heated at 80° C. while being stirred for 30 minutes, and water (150 mL) and ethanol (150 mL) were added thereto, followed by filtration while being heated. The filtrate was concentrated under reduced pressure, and the formed precipitates were recovered through filtration. The thus-obtained solid was washed with ethanol and diisopropyl ether, followed by drying, whereby the title compound (8.5 g) was yielded.

後処理

  1. filtrationfollowed by filtration
  2. temperaturewhile being heated
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe formed precipitates
  5. filtrationwere recovered through filtration
  6. washThe thus-obtained solid was washed with ethanol and diisopropyl ether
  7. customby drying

出典と根拠

ORDレコード
ord-d1d3c7e6655740a5bd30cf0e49dcf14e
出典データセット
uspto-grants-2013_08
特許番号
US08501772B2

反応ノート

読み込み中…