Lithium Hydroxide → HCID 21844877, 화합물

HRID 618910

반응식

HRID 618910 반응식
[NH:1]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:13]([CH:20](Br)[C:21]([OH:23])=[O:22])[CH2:14][CH:15](Br)[C:16]([OH:18])=[O:17].[OH-].[Li+]>O>[N:1]1([CH:15]([CH2:14][CH2:13][CH:20]([N:1]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[C:21]([OH:23])=[O:22])[C:16]([OH:18])=[O:17])[CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 649631,4,7,10-TetraazacyclododecaneHCID 998602,5-Dibromoadipic acid

생성물 1

HCID 21844877HCID 21844877, 화합물수율 51.8%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

A mixture of cyclen (60.75 g, 350 mmol), meso-2,5-dibromoadipic acid (10.57 g, 35 mmol), and 1M lithium hydroxide (70 mL, 70 mmol) in water (104 mL) was heated to 60° C. under nitrogen for 170 hours. After cooling to ambient temperature, the reaction mixture was applied to an AG1X8 anion exchange column [400 mL (OH-form)]. The column was washed thoroughly with water (4 L), and the product was eluted with 0.5M acetic acid (2 L). Fractions containing product were combined, chased with water (3×200 mL) and ethanol (3×100 mL) to yield the title product (8.75 g, 51.8%) as a white, hygroscopic foam. Unreacted cyclen was reclaimed by concentration of the first 2 L of eluent and recrystallization from water. 1H NMR: (D2O) δ 2.75-2.90 (br mult, 34H), 1.52 (br, 4H). 13C NMR: (D2O) 24.3, 40.5, 41.1, 41.3, 41.6, 43.1, 44.9, 63.0, 177.1. MS (FAB): m/e 487.4 (MH+).

후처리

  1. temperatureAfter cooling to ambient temperature
  2. washThe column was washed thoroughly with water (4 L)
  3. washthe product was eluted with 0.5M acetic acid (2 L)
  4. additionFractions containing product

출처 및 근거

ORD 기록
ord-a07b91f93c0e440ca4be97a435d3f3a0
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958373

연결된 노트

불러오는 중…