Carbonyl biscaprolactam → 4-(Isocyanatomethyl) nonane

HRID 1279680노트

반응식

HRID 1279680 반응식
[C:1]([CH:11]1[NH:18][C:16](=[O:17])CCCC1)([CH:3]1NC(=O)[CH2:7][CH2:6][CH2:5][CH2:4]1)=O.N[C:20](N)(N)[CH2:21][CH2:22]CCCCCC>C(OCC)(=O)C>[N:18]([CH2:11][CH:1]([CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])[CH2:20][CH2:21][CH3:22])=[C:16]=[O:17]

참가 물질

4

반응물 2

HCID 10377529Carbonyl biscaprolactamHCID 18954154Triamino nonane

생성물 1

HCID 184289794-(Isocyanatomethyl) nonane

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

302.4 g (1.2 mol) carbonyl-bis-caprolactam was dissolved in 400 ml ethyl acetate at 78° C. In one hour 69.3 g (0.4 mol) triamino nonane, dissolved in 100 ml ethyl acetate, was added dropwise. The reaction was monitored by means of TLC. After 3 hours the clear solution was cooled to room temperature and extracted 4 times with 500 ml water (with some NaCl). The solution was then dried with NaSO4. The NaSO4 was removed by filtration and the ethyl acetate was removed by means of the rotavapor. The product was dried at 75° C. and in a vacuum. Caprolactam-blocked of 1,8-diisocyanato, 4-(isocyanatomethyl) nonane was obtained pure, as a lightly coloured oil (yield=99%).

후처리

  1. additionwas added dropwise
  2. extractionextracted 4 times with 500 ml water (with some NaCl)
  3. dry with materialThe solution was then dried with NaSO4
  4. customThe NaSO4 was removed by filtration
  5. customthe ethyl acetate was removed by means of the rotavapor
  6. customThe product was dried at 75° C. and in a vacuum

출처 및 근거

ORD 기록
ord-1ec9b015992a442e83894665ba943d41
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06448394B1

반응 노트

불러오는 중…