Carbonyl biscaprolactam → 4-(Isocyanatomethyl) nonane

HRID 1279680ノート

反応式

HRID 1279680 の反応式
[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]

参加物

4

反応物 2

HCID 10377529Carbonyl biscaprolactamHCID 18954154Triamino nonane

生成物 1

HCID 184289794-(Isocyanatomethyl) nonane

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-1ec9b015992a442e83894665ba943d41
出典データセット
uspto-grants-2002_09
特許番号
US06448394B1

反応ノート

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