Hydrochloric Acid → N-(2-aminopropyl)propane-1,2-diamine

HRID 571596

반응식

HRID 571596 반응식
[NH2:1][CH2:2][CH:3]([NH2:5])[CH3:4].Cl.[CH3:7][CH:8]1[CH2:10][NH:9]1>O>[NH2:5][CH:3]([CH3:4])[CH2:2][NH:1][CH2:7][CH:8]([NH2:9])[CH3:10]

참가 물질

5

반응 조건

온도
110 °C

실험 절차

Into a 500 mL flask, 180 mL of de-ionized water was placed. To this, 120 mL of 1,2-diaminopropane (1.39 mol) was added and a condenser was fitted to the flask. 50 mL (0.507 mol) of hydrogen chloride (37%) was added dropwise and the reaction allowed to subside before adding 10 mL of 2-methylaziridine (0.142 mol). The solution was then heated to 110° C. for 25 hours. The solvent and excess 1,2-diaminopropane were then removed by vacuum distillation. The crude product was then distilled under vacuum (approximately 40 torr) with a boiling point of 110° C. The yield was 24% with 4.541 g obtained. The purity was determined by NMR, showing multiplets at 2.71, 2.35 and 0.91 ppm which corresponded to those in a commercial sample. There was an additional peak at 2.11 ppm which may be due to a structural isomer of the product.

후처리

  1. customa condenser was fitted to the flask
  2. customThe solvent and excess 1,2-diaminopropane were then removed by vacuum distillation
  3. distillationThe crude product was then distilled under vacuum (approximately 40 torr) with a boiling point of 110° C
  4. customThe yield was 24% with 4.541 g obtained

출처 및 근거

ORD 기록
ord-058266bcc3c143fbb63f34bba87704bd
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029189B2

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