5-Nitroisophthaloyl chloride → 2'-Methyl-5-nitro-5'-(4,6,8-trisulfo-1-naphthylcarbamoyl)isophthalanilic acid

HRID 2052468ノート

反応式

HRID 2052468 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:13](Cl)=[O:14])[CH:7]=C([CH:12]=1)C(Cl)=O)([O-:3])=[O:2].N[C:17]1[CH:18]=[C:19]([CH3:48])[CH:20]=[CH:21][C:22]=1[C:23]([NH:25][C:26]1[C:35]2[C:34]([S:36]([OH:39])(=[O:38])=[O:37])=[CH:33][C:32]([S:40]([OH:43])(=[O:42])=[O:41])=[CH:31][C:30]=2[C:29]([S:44]([OH:47])(=[O:46])=[O:45])=[CH:28][CH:27]=1)=[O:24].C1C([N:55]=NC2C(=O)N(C3C=CC(S([O-])(=O)=O)=CC=3)N=C2C([O-])=O)=CC=C(S([O-])(=O)=O)C=1.[Na+].[Na+].[Na+].O.O.O.[C:86]([O-:89])(=[O:88])[CH3:87].[Na+]>CCOCC.O>[CH3:48][C:19]1[CH:18]=[CH:17][C:22]([C:23](=[O:24])[NH:25][C:26]2[C:35]3[C:30](=[CH:31][C:32]([S:40]([OH:43])(=[O:42])=[O:41])=[CH:33][C:34]=3[S:36]([OH:39])(=[O:37])=[O:38])[C:29]([S:44]([OH:47])(=[O:45])=[O:46])=[CH:28][CH:27]=2)=[CH:21][C:20]=1[NH:55][C:13](=[O:14])[C:6]1[CH:7]=[C:87]([CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)[C:86]([OH:89])=[O:88]

参加物

7

反応物 4

HCID 834515-Nitroisophthaloyl chlorideHCID 164825TartrazineHCID 23665404Sodium Acetate TrihydrateHCID 570945898(3-Amino-p-toluamido)-1,3,5-naphthalenetrisulfonic acid

生成物 1

HCID 203767912'-Methyl-5-nitro-5'-(4,6,8-trisulfo-1-naphthylcarbamoyl)isophthalanilic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 2.78 g of 5-nitroisophthaloyl chloride in 50 ml of ether is added to a stirred mixture of 6.5 g of 8-(3-amino-p-toluamido)-1,3,5-naphthalenetrisulfonic acid, trisodium salt, 3.2 g of sodium acetate trihydrate, 50 ml of water and 40 ml of ether over a 40 minute period. The mixture is stirred for an additional 30 minutes, then is evaporated. The residue is dissolved in 20 ml of hot water, then is placed in an icebox overnight. The precipitate is collected, washed with ice-water, 80% aqueous ethanol, ethanol and ether and is dried to yield 2.9 g of 2'-methyl-5-nitro-5'-(4,6,8-trisulfo-1-naphthylcarbamoyl)isophthalanilic acid, trisodium salt.

後処理

  1. customis evaporated
  2. dissolutionThe residue is dissolved in 20 ml of hot water
  3. waitis placed in an icebox overnight
  4. customThe precipitate is collected
  5. washwashed with ice-water, 80% aqueous ethanol, ethanol and ether
  6. customis dried

出典と根拠

ORDレコード
ord-f3aa20de38694568800f326f438cb238
出典データセット
uspto-grants-1980_01
特許番号
US04185033

反応ノート

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