Ammonia → 7-Nitro-5-pyridin-3-yl-benzothiazol-2-ylamine

HRID 1010653ノート

反応式

HRID 1010653 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:16]2[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=2)[CH:7]=[C:8]([N+:13]([O-])=O)[C:9]=1[S:10][C:11]#[N:12])([O-:3])=[O:2].N>C(O)(=O)C.O.[Fe]>[N+:1]([C:4]1[C:9]2[S:10][C:11]([NH2:12])=[N:13][C:8]=2[CH:7]=[C:6]([C:16]2[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=2)[CH:5]=1)([O-:3])=[O:2]

参加物

6

反応物 2

HCID 222AmmoniaHCID 578136843-(3,5-Dinitro-4-thiocyanato-phenyl)-pyridine

生成物 1

HCID 578137647-Nitro-5-pyridin-3-yl-benzothiazol-2-ylamine収率 95.6%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A solution of 3-(3,5-Dinitro-4-thiocyanato-phenyl)-pyridine (0.66 g, 2.19 mmol) in glacial acetic acid (15 ml) was treated with iron powder (0.61 g, 11.0 mmol) and stirred at ambient temperature for 16 h. The resultant mixture was diluted with water (200 ml) and made alkaline by the addition of concentrated ammonia solution. The solid material was collected by filtration and washed with water followed by ethyl acetate. The filtered solid was then extracted with boiling ethanol (3×200 ml) which was removed in vacuo to give 7-Nitro-5-pyridin-3-yl-benzothiazol-2-ylamine as a pale yellow solid (0.57 g, 95%).

後処理

  1. filtrationThe solid material was collected by filtration
  2. washwashed with water
  3. extractionThe filtered solid was then extracted with boiling ethanol (3×200 ml) which
  4. customwas removed in vacuo

出典と根拠

ORDレコード
ord-ee0671df6b3b454e811b6b6ee6b89e11
出典データセット
uspto-grants-2011_07
特許番号
US07977340B2

反応ノート

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