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4-nitro-N-ethylphthalimide → 5-Amino-2-ethylisoindoline-1,3-dione

HRID 2288128
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HRID 2288128 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[O:12])[N:10]([CH2:13][CH3:14])[C:8](=[O:9])[C:7]2=[CH:15][CH:16]=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][CH3:14])[C:8](=[O:9])[C:7]2=[CH:15][CH:16]=1
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참가 물질

7

반응물 2

HCID 8404084-nitro-N-ethylphthalimide2회HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 187040545-Amino-2-ethylisoindoline-1,3-dione수율 84.2%

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 62684Vanadic acid, ammonium salt촉매
HCID 162651
Titanium oxide (Ti3O)
촉매
HCID 962Water용매

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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 2.2 g of 4-nitro-N-ethylphthalimide. After displacing the air with nitrogen, the latter is replaced by hydrogen at atmospheric pressure and the suspension is stirred at 65° C. for 42 hours. During this time, 95% of the theoretical amount of hydrogen, based on the 4-nitro-N-ethylphthalimide, 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 1.6 g (84%) of 4-amino-N-ethylphthalimide.

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-f07a7023e17a40659fa8378fbe3edb75
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06087480

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