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5-Nitroisophthaloyl chloride → 8,8'-[(5-Nitro-1,3-phenylene)bis(carbonylimino)]-di-1,3,6-naphthalenetrisulfonic acid hexasodium salt

HRID 867136
ノート
印刷プレビュー

反応式

HRID 867136 の反応式
[Na+:1].[Na+].[Na+].[NH2:4][C:5]1[CH:6]=[C:7]([S:23]([O-:26])(=[O:25])=[O:24])[CH:8]=[C:9]2[C:14]=1[C:13]([S:15]([O-:18])(=[O:17])=[O:16])=[CH:12][C:11]([S:19]([O-:22])(=[O:21])=[O:20])=[CH:10]2.[OH2:27].[OH2:28].[OH2:29].[C:30]([O-])(=O)[CH3:31].[Na+].[N+:35]([C:38]1[CH:39]=[C:40]([C:47](Cl)=[O:48])[CH:41]=[C:42]([CH:46]=1)[C:43](Cl)=[O:44])([O-:37])=[O:36]>O>[Na+:1].[Na+:1].[Na+:1].[Na+:1].[Na+:1].[Na+:1].[N+:35]([C:38]1[CH:39]=[C:40]([C:47]([NH:4][C:5]2[CH:6]=[C:7]([S:23]([O-:26])(=[O:24])=[O:25])[CH:8]=[C:31]3[C:30]=2[C:11]([S:19]([O-:29])(=[O:28])=[O:27])=[CH:12][C:13]([S:15]([O-:18])(=[O:16])=[O:17])=[CH:14]3)=[O:48])[CH:41]=[C:42]([C:43]([NH:4][C:5]2[CH:6]=[C:7]([S:23]([O-:26])(=[O:25])=[O:24])[CH:8]=[C:9]3[C:14]=2[C:13]([S:15]([O-:18])(=[O:17])=[O:16])=[CH:12][C:11]([S:19]([O-:22])(=[O:20])=[O:21])=[CH:10]3)=[O:44])[CH:46]=1)([O-:37])=[O:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 834515-Nitroisophthaloyl chlorideHCID 1018991,3,6-Naphthalenetrisulfonic acid, 8-amino-, sodium salt (1:?)HCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 1317111748,8'-[(5-Nitro-1,3-phenylene)bis(carbonylimino)]-di-1,3,6-naphthalenetrisulfonic acid hexasodium salt収率 252%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

To a solution of 13.75 g of 8-amino-1,3,6-naphthalenetrisulfonic acid trisodium salt and 4.6 g of sodium acetate trihydrate in 100 ml of water in a 500 ml baffle flask is added 4.10 g of powdered 5-nitroisophthaloyl chloride. The mixture is stirred vigorously at room temperature for one hour then is filtered through diatomaceous earth. The filtrate is concentrated to 50 ml, then warmed, acidified with 0.5 ml of concentrated hydrochloric acid and diluted with 50 ml of hot ethanol. The product is crystallized on cooling with scratching and is collected by filtration, then washed with 25 ml of 55% aqueous ethanol and 60 ml of ethanol. Additional product is obtained from the filtrate in the same manner. The total product is dried by conventional means to give 13.8 g of 8,8'-[(5-nitro-1,3-phenylene)bis(carbonylimino)]-di-1,3,6-naphthalenetrisulfonic acid hexasodium salt.

後処理

  1. filtrationthen is filtered through diatomaceous earth
  2. concentrationThe filtrate is concentrated to 50 ml
  3. temperaturewarmed
  4. additiondiluted with 50 ml of hot ethanol
  5. customThe product is crystallized
  6. temperatureon cooling
  7. filtrationis collected by filtration
  8. washwashed with 25 ml of 55% aqueous ethanol and 60 ml of ethanol
  9. customAdditional product is obtained from the filtrate in the same manner
  10. customThe total product is dried by conventional means

出典と根拠

ORDレコード
ord-75d668475828472f91af17412ff87d3e
出典データセット
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04102917

反応ノート

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