8-[4-(4-Nitro-2-sulfobenzamido)-2-sulfobenzamido]-1,3,6-naphthalenetrisulfonic acid → 8-[4-(4-Amino-2-sulfobenzamido)-2-sulfobenzamido]-1,3,6-naphthalenetrisulfonic acid

HRID 2166509ノート

反応式

HRID 2166509 の反応式
[N+:1]([C:4]1[CH:47]=[CH:46][C:7]([C:8]([NH:10][C:11]2[CH:41]=[CH:40][C:14]([C:15]([NH:17][C:18]3[CH:19]=[C:20]([S:36]([OH:39])(=[O:38])=[O:37])[CH:21]=[C:22]4[C:27]=3[C:26]([S:28]([OH:31])(=[O:30])=[O:29])=[CH:25][C:24]([S:32]([OH:35])(=[O:34])=[O:33])=[CH:23]4)=[O:16])=[C:13]([S:42]([OH:45])(=[O:44])=[O:43])[CH:12]=2)=[O:9])=[C:6]([S:48]([OH:51])(=[O:50])=[O:49])[CH:5]=1)([O-])=O>[Pd].O>[NH2:1][C:4]1[CH:47]=[CH:46][C:7]([C:8]([NH:10][C:11]2[CH:41]=[CH:40][C:14]([C:15]([NH:17][C:18]3[CH:19]=[C:20]([S:36]([OH:39])(=[O:37])=[O:38])[CH:21]=[C:22]4[C:27]=3[C:26]([S:28]([OH:31])(=[O:29])=[O:30])=[CH:25][C:24]([S:32]([OH:35])(=[O:34])=[O:33])=[CH:23]4)=[O:16])=[C:13]([S:42]([OH:45])(=[O:43])=[O:44])[CH:12]=2)=[O:9])=[C:6]([S:48]([OH:51])(=[O:50])=[O:49])[CH:5]=1

参加物

4

実験手順

A reaction mixture comprising 17.5 g of 8-[4-(4-nitro-2-sulfobenzamido)-2-sulfobenzamido]-1,3,6-naphthalenetrisulfonic acid, pentasodium salt, 1.0 g of 10% palladium on carbon catalyst and 100 ml of water was hydrogenated in a Parr shaker for one hour and then filtered through diatomaceous earth. The filtrate was concentrated to about 65 ml and then poured with vigorous stirring into 500 ml of absolute ethanol. The granular precipitate was collected by filtration, washed with ethanol, then ether and dried for three days at 110° C., giving 8-[4-(4-amino-2-sulfobenzamido)-2-sulfobenzamido]-1,3,6-naphthalenetrisulfonic acid, pentasodium salt.

後処理

  1. filtrationfiltered through diatomaceous earth
  2. concentrationThe filtrate was concentrated to about 65 ml
  3. additionpoured
  4. filtrationThe granular precipitate was collected by filtration
  5. washwashed with ethanol
  6. dry with materialether and dried for three days at 110° C.

出典と根拠

ORDレコード
ord-06d4d3a6771d43c0b1255f74ef3e12fb
出典データセット
uspto-grants-1983_06
特許番号
US04387059

反応ノート

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