1,3,5-trimethoxy-2,4-dinitrobenzene → HCID 23009735、化合物

HRID 359638ノート

反応式

HRID 359638 の反応式
[N+:1]([C:4]1[C:9]([O:10][CH3:11])=[C:8]([N+:12]([O-])=O)[C:7]([O:15][CH3:16])=[CH:6][C:5]=1[O:17][CH3:18])([O-:3])=[O:2].[PH2]([O-])=O.[Na+]>[Pd].O1CCCC1.O>[NH2:12][C:8]1[C:9]([O:10][CH3:11])=[C:4]([N+:1]([O-:3])=[O:2])[C:5]([O:17][CH3:18])=[CH:6][C:7]=1[O:15][CH3:16]

参加物

6

反応物 2

HCID 27749591,3,5-trimethoxy-2,4-dinitrobenzeneHCID 178527019HCID 178527019、化合物

生成物 1

HCID 23009735HCID 23009735、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of 26 g of palladium on charcoal (10%) is refluxed in 1.3 l of tetrahydrofuran and 26 ml of water containing 1 mole (258 g) of 2,4-dinitro-1,3,5-trimethoxybenzene. A solution of 247 g of sodium hypophosphite in 260 ml of water is added to this suspension over 3 hours. Refluxing is continued for an additional 30 minutes. After cooling, the catalyst is removed by filtration and the aqueous phase by phase separation. The organic phase is concentrated under vacuum and is then poured onto ice. The expected product precipitates. It melts at 111° C.

後処理

  1. temperatureRefluxing
  2. temperatureAfter cooling
  3. customthe catalyst is removed by filtration
  4. customthe aqueous phase by phase separation
  5. concentrationThe organic phase is concentrated under vacuum
  6. additionis then poured onto ice
  7. customThe expected product precipitates

出典と根拠

ORDレコード
ord-53212ae6178b46fab4b2a15b4a3f3c7b
出典データセット
uspto-grants-1991_03
特許番号
US05002585

反応ノート

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