HRID2052469

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：O=C([O-])C1=NN(c2ccc(S(=O)(=O)[O-])cc2)C(=O)C1N=Nc1ccc(S(=O)(=O)[O-])cc1.[Na+].[Na+].[Na+]

HCID164825

未命名化合物

HCID23665404

Sodium Acetate Trihydrate

C2H9NaO5

结构：O=C(OC(=O)c1ccc([N+](=O)[O-])cc1S(=O)(=O)O)c1ccc([N+](=O)[O-])cc1S(=O)(=O)O

HCID57002923

未命名化合物

结构：Cc1ccc(C(=O)Nc2ccc(S(=O)(=O)O)c3cc(S(=O)(=O)O)cc(S(=O)(=O)O)c23)c(N)c1

HCID57094589

未命名化合物

PRODUCTS

生成物

结构：Cc1ccc(C(=O)Nc2ccc(S(=O)(=O)O)c3cc(S(=O)(=O)O)cc(S(=O)(=O)O)c23)c(NC(=O)c2ccc([N+](=O)[O-])cc2S(=O)(=O)O)c1

HCID57162934

未命名化合物

收率 87.4%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

To a stirred solution of 6.5 g of 8(3-amino-p-toluamido)-1,3,5-naphthalenetrisulfonic acid, trisodium salt (prepared in Example 1) and 2.4 g of sodium acetate trihydrate in 43.0 ml of water is added 3.07 g of 4-nitro-2-sulfobenzoic acid anhydride. The mixture is stirred for 30 minutes then is filtered. The filtrate is acidified with 0.98 ml of concentrated hydrochloric acid and evaporated in vacuo. The residue is dissolved in 20 ml of hot water which is added to 130 ml of absolute ethanol forming a gelatinous precipitate. The material is collected and washed with 80% aqueous ethanol, ethanol and ether and is dried to yield 4.2 g of 8-[3-(4-nitro-2-sulfobenzamido)-p-toluamido]-1,3,5-naphthalenetrisulfonic acid, tetrasodium salt.

WORKUP

后处理

filtrationthen is filtered
customevaporated in vacuo
dissolutionThe residue is dissolved in 20 ml of hot water which
additionis added to 130 ml of absolute ethanol forming a gelatinous precipitate
customThe material is collected
washwashed with 80% aqueous ethanol, ethanol and ether
customis dried

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-a0859022a6804315b3fea7d064a0a53c
来源数据集: uspto-grants-1980_01
DOI: 10.6084/m9.figshare.5104873.v1
专利: US04185033
来源说明: uspto-grants-1980_01

反应 SMILES

[NH2:1][C:2]1[CH:3]=[C:4]([CH3:33])[CH:5]=[CH:6][C:7]=1[C:8]([NH:10][C:11]1[C:20]2[C:19]([S:21]([OH:24])(=[O:23])=[O:22])=[CH:18][C:17]([S:25]([OH:28])(=[O:27])=[O:26])=[CH:16][C:15]=2[C:14]([S:29]([OH:32])(=[O:31])=[O:30])=[CH:13][CH:12]=1)=[O:9].C1C(N=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([O-])(=O)C.[Na+].[N+](C1C=CC(C([O:85][C:86](=O)[C:87]2[CH:92]=[CH:91][C:90]([N+:93]([O-:95])=[O:94])=[CH:89][C:88]=2[S:96]([OH:99])(=[O:98])=[O:97])=O)=C(S(O)(=O)=O)C=1)([O-])=O>O>[N+:93]([C:90]1[CH:91]=[CH:92][C:87]([C:86]([NH:1][C:2]2[CH:3]=[C:4]([CH3:33])[CH:5]=[CH:6][C:7]=2[C:8]([NH:10][C:11]2[C:20]3[C:19]([S:21]([OH:24])(=[O:23])=[O:22])=[CH:18][C:17]([S:25]([OH:28])(=[O:26])=[O:27])=[CH:16][C:15]=3[C:14]([S:29]([OH:32])(=[O:31])=[O:30])=[CH:13][CH:12]=2)=[O:9])=[O:85])=[C:88]([S:96]([OH:99])(=[O:97])=[O:98])[CH:89]=1)([O-:95])=[O:94]