2-Butyl-5-nitro-1H-isoindole-1,3(2H)-dione → 4-amino-N-butylphthalimide

HRID 2288129

반응식

HRID 2288129 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[O:12])[N:10]([CH2:13][CH2:14][CH2:15][CH3:16])[C:8](=[O:9])[C:7]2=[CH:17][CH:18]=1)([O-])=O.[H][H]>N.O[V](=O)=O.[O-2].[O-2].[Ti+4].[Pd].O>[NH2:1][C:4]1[CH:5]=[C:6]2[C:11](=[O:12])[N:10]([CH2:13][CH2:14][CH2:15][CH3:16])[C:8](=[O:9])[C:7]2=[CH:17][CH:18]=1

참가 물질

7

반응물 2

HCID 932972-Butyl-5-nitro-1H-isoindole-1,3(2H)-dione2회HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 3289774-amino-N-butylphthalimide수율 80%

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 62684Ammonium metavanadate [UN2859] [Poison]촉매HCID 162651Titanium oxide (Ti3O)촉매HCID 962Water용매

반응 조건

온도
65 °C

실험 절차

0.001 g of ammonium vanadate and 0.5 g of titanium dioxide extrudate containing 1% by weight of metallic palladium and having a particle size of 3 mm (from Johnson Matthey) are added to a suspension consisting of 50 ml of water and 2.5 g of 4-nitro-N-butylphthalimide. After displacing the air with nitrogen, the latter is replaced by hydrogen at atmospheric pressure and the suspension is stirred at 65° C. for 68 hours. During this time, 97% of the theoretical amount of hydrogen, based on the 4-nitro-N-butylphthalimide, is absorbed. The resulting suspension is then sieved through a sieve having a mesh width of 1 mm. The material remaining on the sieve is washed with 50 ml of water and the combined aqueous phases are then filtered through a paper filter and washed with 250 ml of water. Drying at 80° C. under reduced pressure (125 mbar) gives 1.7 g (80%) of 4-amino-N-butylphthalimide.

후처리

  1. additionare added to a suspension
  2. customis absorbed
  3. filtrationThe resulting suspension is then sieved through a sieve
  4. washis washed with 50 ml of water
  5. filtrationthe combined aqueous phases are then filtered through a paper
  6. filtrationfilter
  7. washwashed with 250 ml of water
  8. customDrying at 80° C. under reduced pressure (125 mbar)

출처 및 근거

ORD 기록
ord-33c45314607a4e31a3da98e6d2497b13
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06087480

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