Sodium Hydroxide → 1,4-Bis(m-carboxyphenylsulfonyl)-2,5-dimethylpiperazine

HRID 437732

反応式

HRID 437732 の反応式
[CH3:1][C@H:2]1[CH2:7][NH:6][C@H:5]([CH3:8])[CH2:4][NH:3]1.Cl[S:10]([C:13]1[CH:14]=[C:15]([CH:19]=[CH:20][CH:21]=1)[C:16]([OH:18])=[O:17])(=[O:12])=[O:11].[OH-:22].[Na+]>O>[C:16]([C:15]1[CH:14]=[C:13]([S:10]([N:3]2[CH2:4][CH:5]([CH3:8])[N:6]([S:10]([C:13]3[CH:21]=[CH:20][CH:19]=[C:15]([C:16]([OH:18])=[O:17])[CH:14]=3)(=[O:11])=[O:22])[CH2:7][CH:2]2[CH3:1])(=[O:12])=[O:11])[CH:21]=[CH:20][CH:19]=1)([OH:18])=[O:17]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 2206722,5-Dimethylpiperazine, trans-

生成物 1

HCID 214268161,4-Bis(m-carboxyphenylsulfonyl)-2,5-dimethylpiperazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Binder 15 was prepared as follows: Trans-2,5-dimethylpiperazine in water at 50° C. was treated with slightly more than two molar equivalents of m-chlorosulfonylbenzoic acid and five molar equivalents of aqueous sodium hydroxide. Acidification gave 1,4-bis(m-carboxyphenylsulfonyl)-2,5-dimethylpiperazine which was recrystallized from aqueous ethanol. The dimethyl ester was made by boiling the acid for 24 hours in methanol to which some hydrogen chloride has been added. Recrystallization from 2:1 dioxane: water gave a product which melted at 223°-227° C. Anal. Calc'd for C22H26N2O8S2 : C, 51.7; H, 5.1; N, 5.5. Found: C, 51.6; H, 5.4; N, 5.7. The polymer was then made from this ester and ethylene glycol as described for Binder 6.

後処理

  1. customBinder 15 was prepared

出典と根拠

ORDレコード
ord-a7ecdcd3e92647caa616e5f9ba1ee681
出典データセット
uspto-grants-1977_06
特許番号
US04032344

関連ノート

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