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Sulfuric Acid → 2,4,5-Tris(4'-aminophenyl)thiazole

HRID 64993
ノート
印刷プレビュー

反応式

HRID 64993 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[S:11][C:12]([C:24]3[CH:29]=[CH:28][C:27]([N+:30]([O-])=O)=[CH:26][CH:25]=3)=[C:13]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][CH:16]=3)[N:14]=2)=[CH:6][CH:5]=1)([O-])=O.CN(C)C=O.S(=O)(=O)(O)O.C(=O)([O-])O.[Na+]>[Fe].O>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([C:10]2[S:11][C:12]([C:24]3[CH:29]=[CH:28][C:27]([NH2:30])=[CH:26][CH:25]=3)=[C:13]([C:15]3[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=3)[N:14]=2)=[CH:8][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 6228DimethylformamideHCID 516892Sodium BicarbonateHCID 202347972,4,5-Tris(4'-nitrophenyl)thiazole

生成物 1

HCID 202347962,4,5-Tris(4'-aminophenyl)thiazole

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 962
Water
溶媒

反応条件

温度
100 °C

実験手順

15 g (0.034 mol) of the thus obtained 2,4,5-tris(4'-nitrophenyl)thiazole was mixed with 500 ml of N,N-dimethylformamide and 20 g of iron powder. The mixture was admixed with 10 ml of concentrated sulfuric acid and 30 ml of water. The admixture was heated to a temperature of 100° C. with thorough stirring. After 1 hour passed, the solution was neutralized with a saturated aqueous solution of sodium hydrogencarbonate with the reaction temperature kept at 100° C. to adjust the pH value thereof to 8. The reaction solution was then hot-filtered. The filtrate was poured into 3 l of ice water to produce a light yellow precipitate of 2,4,5-tris(4'-aminophenyl)thiazole which was then filtered off and dried to obtain 11.3 g (yield: 94%) of the product.

後処理

  1. customkept at 100° C.
  2. filtrationThe reaction solution was then hot-filtered
  3. additionThe filtrate was poured into 3 l of ice water

出典と根拠

ORDレコード
ord-5b1baca8eea241458711d6cdbea52488
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04612271

反応ノート

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