Phthalic Anhydride → HCID 131718923、化合物

HRID 1608914

反応式

HRID 1608914 の反応式
[NH2:1][C:2]1C=[C:4]2[C:9](=[CH:10][CH:11]=1)C(S(O)(=O)=O)=CC=C2.[C:16]1(=[O:26])[O:21][C:19](=O)[C:18]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:17]12.[Na+].[NH2:28][C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[C:35]([S:39]([O-:42])(=[O:41])=[O:40])=[CH:34][CH:33]=[CH:32]2.C([NH+](CC)CC)C>N1C=CC=CC=1>[NH+:1]1[CH:2]=[CH:11][CH:10]=[CH:9][CH:4]=1.[C:19]1(=[O:21])[N:28]([C:29]2[CH:30]=[C:31]3[C:36](=[CH:37][CH:38]=2)[C:35]([S:39]([O-:42])(=[O:40])=[O:41])=[CH:34][CH:33]=[CH:32]3)[C:16](=[O:26])[C:17]2=[CH:25][CH:24]=[CH:23][CH:22]=[C:18]12

参加物

6

反応物 4

HCID 6811Phthalic AnhydrideHCID 664706-Aminonaphthalene-1-sulphonic acidHCID 1385867TriethylammoniumHCID 23696805Sodium 6-aminonaphthalene-1-sulphonate

生成物 1

HCID 131718923HCID 131718923、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

223 g (1 mol) of 6-amino-1-naphthalenesulfonic acid and 148 g (1 mol) of phthalic anhydride are boiled for 0.5 h in 1 liter of pyridine. After boiling, the reaction mixture is left at room temperature for 16 h. The precipitated product is filtered and washed with pyridine and water, and then recrystallized from boiling water. Yield 298 g (69%); mp 234°-237° C.; Anal. Calcd. for C23H16N2SO5 :C 63.88, H 3.73, N 6.48, S 7.42; Found:C 63.74, H 3.81, N 6.52, S 6.99. When the 6-phthalimido-1-naphthalenesulfonic acid pyridinium salt was synthesized starting from 6-amino-1-naphthalenesulfonic acid sodium salt or triethylammonium salt, the calculated yields were 63% and 58% respectively.

後処理

  1. filtrationThe precipitated product is filtered
  2. washwashed with pyridine and water
  3. customrecrystallized
  4. customthe calculated yields

出典と根拠

ORDレコード
ord-05251847db624057a3846b096fcc6b76
出典データセット
uspto-grants-1995_03
特許番号
US05399487

関連ノート

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