2,5-Dihydroxyterephthalic acid → HCID 178507916、化合物

HRID 1488718

反応式

HRID 1488718 の反応式
[NH2:1][C:2]1[C:3]([NH2:10])=[C:4]([NH2:9])[C:5]([NH2:8])=[N:6][CH:7]=1.O[C:12]1[CH:20]=[C:19]([C:21]([OH:23])=[O:22])[C:18]([OH:24])=[CH:17][C:13]=1[C:14]([OH:16])=[O:15].[NH2:25][C:26]1[C:27]([NH2:34])=[C:28]([NH2:33])[C:29]([NH2:32])=[N:30][CH:31]=1.[OH:35]C1C=C(C(O)=O)C(O)=CC=1C(O)=O>>[OH:35][C:17]1[C:18]([OH:24])=[C:19]([CH:20]=[CH:12][C:13]=1[C:14]([O-:16])=[O:15])[C:21]([O-:23])=[O:22].[NH2:10][C:3]1[CH:2]=[CH:7][N+:6]([NH2:25])=[C:5]([NH2:8])[C:4]=1[NH2:9].[NH2:34][C:27]1[CH:26]=[CH:31][N+:30]([NH2:1])=[C:29]([NH2:32])[C:28]=1[NH2:33]

参加物

4

反応物 3

HCID 691312,5-Dihydroxyterephthalic acid2 回HCID 22906208Tetraaminopyridine2 回HCID 69780930Tetraaminopyridine 2,5-dihydroxyterephthalic acid

生成物 1

HCID 178507916HCID 178507916、化合物

実験手順

With vigorous stirring and without the introduction of any air b) was added to a), producing a rich yellow precipitate. After further adiabatic stirring for 5 minutes, the slurry was cooled, with stirring, to about 10° C. and filtered, washed three times with about 250 ml of degassed water and twice with degassed ethanol, all this without the introduction of air, flushed with nitrogen for 45 minutes, and dried at 1 mbar, 50° C. for 18 hours to produce 16.56 grams (which corresponds to a yield of 98.2%) salt of tetraaminopyridine and 2,5-dihydroxyterephthalic acid. This salt showed a 1:1 tetraaminopyridine/2,5-dihydroxyterephthalic acid composition in NMR. It was found possible to polymerise it to very high DP polymer under standard conditions. Storing the salt of tetraaminopyridine and 2,5-dihydroxyterephthalic acid samples under air instead of under nitrogen showed only slow deterioration of its colour.

後処理

  1. additionwas added to a),
  2. customproducing a rich yellow precipitate
  3. stirringAfter further adiabatic stirring for 5 minutes
  4. temperaturethe slurry was cooled
  5. stirringwith stirring, to about 10° C.
  6. filtrationfiltered
  7. washwashed three times with about 250 ml of degassed water
  8. customtwice with degassed ethanol, all this without the introduction of air, flushed with nitrogen for 45 minutes
  9. customdried at 1 mbar, 50° C. for 18 hours
  10. customto produce 16.56 grams (which
  11. customto polymerise it to very high DP polymer under standard conditions

出典と根拠

ORDレコード
ord-71c7aab86776403c898451626d5792e0
出典データセット
uspto-grants-1997_10
特許番号
US05674969

関連ノート

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