Ammonia → 1,4-Benzenedimethanamine

HRID 27671

반응식

HRID 27671 반응식
O1CCCC1.N.[C:7](#[N:16])[C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1.[H][H]>[Co].O>[C:8]1([CH2:7][NH2:16])[CH:15]=[CH:14][C:11]([CH2:12][NH2:13])=[CH:10][CH:9]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 8028TetrahydrofuranHCID 121721,4-DicyanobenzeneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 683151,4-Benzenedimethanamine

시약·촉매·용매 2

HCID 104730Cobalt촉매HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

A stirred autoclave was charged with 400 ml. tetrahydrofuran (THF), 100 ml. ammonia, 50 g. terephthalonitrile (TPN) and 6.0 g. cobalt supported catalyst and various amounts of water. The autoclave was heated to 120° C. Hydrogen was introduced rapidly until the selected pressure was reached. The absorption of hydrogen started immediately and additional hydrogen was added to keep the pressure at the selected level. The course of the reaction was monitored by measuring the volume of hydrogen consumed and by periodic withdrawal of a small sample of the reaction mixture for analysis. When the analysis indicated that all of the terephthalonitrile had reacted, the agitation was stopped and the reactor was cooled rapidly and vented. The reaction mixture was filtered to recover the catalyst and then was flash evaporated to remove solvent. The residual oil was flash distilled at about 100° C. and 0.5 mm Hg. to give practically pure p-xylylene diamine. A small amount of high boiling residue remained in the distillation pot. Results of experiments conducted with various amounts of water and at 1500 and 2500 psig are listed in Table I.

후처리

  1. additionA stirred autoclave was charged with 400 ml
  2. customThe absorption of hydrogen
  3. additionadditional hydrogen was added
  4. customconsumed and by periodic withdrawal of a small sample of the reaction mixture for analysis
  5. customhad reacted
  6. temperaturethe reactor was cooled rapidly
  7. filtrationThe reaction mixture was filtered
  8. customto recover the catalyst
  9. customevaporated
  10. customto remove solvent
  11. distillationdistilled at about 100° C.

출처 및 근거

ORD 기록
ord-7e6cd9f6c5f9464fbaee0cb1ba972c3b
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04222961

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