Nitric Acid → 2-Butyl-5-nitro-1H-isoindole-1,3(2H)-dione

HRID 613771

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HRID 613771 반응식
[N+:1]([O-:4])([OH:3])=[O:2].[CH2:5]([N:9]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:11]2[C:10]1=[O:19])[CH2:6][CH2:7][CH3:8]>>[N+:1]([C:16]1[CH:15]=[C:12]2[C:13](=[O:14])[N:9]([CH2:5][CH2:6][CH2:7][CH3:8])[C:10](=[O:19])[C:11]2=[CH:18][CH:17]=1)([O-:4])=[O:2].[N+:1]([C:15]1[CH:16]=[CH:17][CH:18]=[C:11]2[C:10]([N:9]([CH2:5][CH2:6][CH2:7][CH3:8])[C:13](=[O:14])[C:12]=12)=[O:19])([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 73812N-Butylphthalimide2회

생성물 2

HCID 932972-Butyl-5-nitro-1H-isoindole-1,3(2H)-dioneHCID 45479101H-Isoindole-1,3(2H)-dione, 2-butyl-4-nitro-

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온도
100 °C

실험 절차

A 3-necked, 5-liter round-bottomed flask, equipped with a mechanical stirrer, was charged with 4,259 g (67.6 moles) of 99% nitric acid. To the flask was added 524.9 g (2.58 moles) N-butylphthalimide as a liquid at such a rate as to keep the reaction temperature under 40° C. The addition of the N-butylphthalimide was completed in about a half hour. The reaction was then heated for six hours to 50° C. in a temperature controlled water bath. The reaction product was then fed to a wiped film evaporator that was heated at 100° C. and under vacuum (30 mm). The bulk of the nitric acid was distilled off and the liquid product, i.e., 4-nitro-N-butylphthalimide and 3-nitro-N-butylphthalimide in a ratio of about 25:1, was isolated as a liquid which rapidly solidified to about 98% solids upon cooling in the collection vessel. Depending on the operation of the evaporator, the residual nitric acid in the product was less than 3% by weight, and was as low as 0.1% by weight

후처리

  1. customA 3-necked, 5-liter round-bottomed flask, equipped with a mechanical stirrer
  2. customunder 40° C
  3. waitwas completed in about a half hour
  4. temperatureThe reaction was then heated for six hours to 50° C. in a temperature
  5. customThe reaction product was then fed to a wiped film evaporator that
  6. distillationThe bulk of the nitric acid was distilled off

출처 및 근거

ORD 기록
ord-3c82667ae3fc43feb3ee48a5615550fd
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06008374

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