Water → 1H-Pyrrole-2,5-dione, 1-dodecyl-

HRID 868687

반응식

HRID 868687 반응식
O.[C:2]1(=[O:8])O[C:5](=[O:6])[CH:4]=[CH:3]1.[CH2:9]([NH2:21])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].P(=O)(O)(O)O>C1(C)C(C)=CC=CC=1>[CH2:9]([N:21]1[C:5](=[O:6])[CH:4]=[CH:3][C:2]1=[O:8])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]

참가 물질

6

반응물 4

HCID 962WaterHCID 1004Phosphoric AcidHCID 7923Maleic AnhydrideHCID 13583Dodecylamine

생성물 1

HCID 871911H-Pyrrole-2,5-dione, 1-dodecyl-

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

반응 조건

온도
215 °C

실험 절차

A glass flask having an inner volume of 3 liters was fitted with a thermometer, a stirrer, and a water separator. In this reactor, 240 g of a solution containing 120 g of maleic anhydride in xylene was placed. Then, a solution containing 220 g of dodecylamine in 1880 g of xylene was added gradually and piecemeal over a period of 120 minutes at 40° C. to the reactor. After the addition was completed, the mixture in the reactor and 65.4 g of orthophosphoric acid (purity 89% by weight) added thereto were heated at 215° C. for 1 hour under 4.4 kg/cm2. G to effect reaction. The resultant reaction mixture was cooled to 30° C., washed with 400 ml of water, and separated into a water layer and a xylene layer. The xylene layer was separated by filtration to effect removal of insolubles. The xylene layer was distilled to expel xylene. Consequently, there was obtained 258 g of slightly impure N-dodecyl maleimide. This product was found to have purity of 85.3% by weight, indicating the yield to be 69.9 mol % based on dodecylamine.

후처리

  1. customA glass flask having
  2. customan inner volume of 3 liters was fitted with a thermometer, a stirrer
  3. additionwas added gradually and piecemeal over a period of 120 minutes at 40° C. to the reactor
  4. additionAfter the addition
  5. customreaction
  6. customThe resultant reaction mixture
  7. temperaturewas cooled to 30° C.
  8. washwashed with 400 ml of water
  9. customseparated into a water layer
  10. customThe xylene layer was separated by filtration
  11. customremoval of insolubles
  12. distillationThe xylene layer was distilled

출처 및 근거

ORD 기록
ord-8ca61568373446e98509b7f03ca6cd7a
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780546

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