Water → Caprolactam n-Hexylamine

HRID 28077

반응식

HRID 28077 반응식
[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:9]([NH2:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].O>>[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:9]([NH2:15])[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]

참가 물질

4

반응물 3

HCID 962WaterHCID 7768CaprolactamHCID 8102Hexylamine

생성물 1

HCID 86737235Caprolactam n-Hexylamine

반응 조건

온도
250 °C

실험 절차

A 200-ml. pressure reactor was charged with 50 g. (0.442 mole) of ε-caprolactam (CL), 10 g. (0.099 mole) of n-hexylamine (HA) and 0.2 g. (0.011 mole) of water. The reactor was cooled in a dry ice-acetone bath, evacuatively purged twice with nitrogen, evacuated, and heated at 250° C. for 16 hours with the contents under autogenous pressure. The cooled product was a soft white solid. A 45-g. portion was extracted by centrifugation first with about 900 ml. of 1:1 acetone:water and secondly with acetone. The air-dried residue weighed 25.5 g., and could be readily crushed to a fine powder. Analysis showed 865 equivalents of amino end groups per 106 g., corresponding to a degree of polymerization (DP) of about 9. Differential scanning calorimetry (DSC) showed a major melting endotherm at 196°-198° C.

후처리

  1. additionpressure reactor was charged with 50 g
  2. temperatureThe reactor was cooled in a dry ice-acetone bath
  3. customevacuatively purged twice with nitrogen
  4. customevacuated
  5. extractionportion was extracted by centrifugation first with about 900 ml
  6. custom, and could be readily crushed to a fine powder
  7. custom, corresponding to a degree of polymerization (DP) of about 9
  8. customat 196°-198° C.

출처 및 근거

ORD 기록
ord-25e331e0a5a340eb8acf8cef3c0a59b8
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225476

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