Phosphorus oxide (P4O10) → 1,2,4,5-Benzenetetraamine

HRID 2231955

반응식

HRID 2231955 반응식
Cl.Cl.Cl.Cl.[NH2:5][C:6]1[CH:11]=[C:10]([NH2:12])[C:9]([NH2:13])=[CH:8][C:7]=1[NH2:14].S1C2C=CC=CC=2N=C1C1C(C(O)=O)=CC=C(C(O)=O)C=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[NH2:5][C:6]1[CH:11]=[C:10]([NH2:12])[C:9]([NH2:13])=[CH:8][C:7]=1[NH2:14]

참가 물질

4

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 782601,2,4,5-Benzenetetraamine tetrahydrochlorideHCID 43022361,4-Benzenedicarboxylic acid, 2-(2-benzothiazolyl)-

생성물 1

HCID 782611,2,4,5-Benzenetetraamine

반응 조건

온도
90 °C

실험 절차

1,2,4,5-tetraaminobenzene tetrahydrochloride (1.7138 g, 6.033 mmol), 2-benzothiazole terephthalic acid (1.8059 g, 6.033 mmol) and 5.57 g of polyphosphoric acid (77% P2O5) were placed in a resin flask equipped with a mechanical stirrer, nitrogen inlet/outlet tubes, a vacuum connector and a side opening on the resin flask. The solution was heated at 90° C. in vacuo for 24 hours for dehydrochlorination. The reaction mixture was cooled to 60° C., then 4.04 g of P2O5 was added, in vacuo, thereby raising the polymer concentration to 18%. After adding the P2O5, heating was resumed. The reaction mixture was heated to 164° C., at which temperature the mixture became opalescent. The mixture was heated at 174° C. for 24 hours, then at 190° C. for 4 hours. Work-up, as in the preceeding Example, gave a polymer with [N]=7.5 dl/g, methanesulfonic acid at 30° C.

후처리

  1. customequipped with a mechanical stirrer, nitrogen inlet/outlet tubes
  2. temperatureThe reaction mixture was cooled to 60° C.
  3. temperatureraising
  4. concentrationthe polymer concentration to 18%
  5. additionAfter adding the P2O5
  6. temperatureheating
  7. temperatureThe reaction mixture was heated to 164° C., at which temperature the mixture
  8. temperatureThe mixture was heated at 174° C. for 24 hours
  9. customat 30° C.

출처 및 근거

ORD 기록
ord-aa6ef18ea8434f53b510154735638b59
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04785115

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