Sodium Carbonate → 1-[3-(Triethoxysilyl)propyl]-1,4,8,11-tetraazacyclotetradecane

HRID 842304

반응식

HRID 842304 반응식
[NH:1]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[Na+].[Na+].I[CH2:22][CH2:23][CH2:24][Si:25]([O:32][CH2:33][CH3:34])([O:29][CH2:30][CH3:31])[O:26][CH2:27][CH3:28]>C(#N)C>[CH2:30]([O:29][Si:25]([O:32][CH2:33][CH3:34])([O:26][CH2:27][CH3:28])[CH2:24][CH2:23][CH2:22][N:1]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)[CH3:31]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 649641,4,8,11-TetraazacyclotetradecaneHCID 11782516(3-Iodopropyl)triethoxysilane

생성물 1

HCID 155401471-[3-(Triethoxysilyl)propyl]-1,4,8,11-tetraazacyclotetradecane

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

72 g (0.359 mol) of cyclam and 15 g of Na2CO3 (dried at 100° C. under 1 mm Hg for 24 h) are placed in 2.5 l of acetonitrile in a 6 l reactor under a stream of nitrogen. The mixture is brought to reflux, a solution of 24.2 g (0.073 mol) of iodopropyltriethoxysilane in 500 ml of acetonitrile is then added dropwise and then the reaction mixture is maintained at reflux for 48 h. After evaporating the solvent on a rotary evaporator (still under a nitrogen atmosphere), pentane is added to the residue and the excess cyclam is filtered off. This operation is repeated three times, the filtrates are combined, the pentane is evaporated and compound 1 is obtained in the form of a colorless oil (15 g, 50.8%).

후처리

  1. temperatureto reflux
  2. temperaturethe reaction mixture is maintained
  3. temperatureat reflux for 48 h
  4. customAfter evaporating the solvent
  5. customon a rotary evaporator (still under a nitrogen atmosphere), pentane
  6. additionis added to the residue
  7. filtrationthe excess cyclam is filtered off
  8. customthe pentane is evaporated

출처 및 근거

ORD 기록
ord-0514501f0ef044f991efe7780a814ce4
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06372903B1

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