1,3,5-trimethoxy-2,4-dinitrobenzene → HCID 23009735, 화합물

HRID 359638노트

반응식

HRID 359638 반응식
[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]

참가 물질

6

반응물 2

HCID 27749591,3,5-trimethoxy-2,4-dinitrobenzeneHCID 178527019HCID 178527019, 화합물

생성물 1

HCID 23009735HCID 23009735, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-53212ae6178b46fab4b2a15b4a3f3c7b
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05002585

반응 노트

불러오는 중…