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

HRID 1941944노트

반응식

HRID 1941944 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-32dc04f77aae49d69454401b81f3a7e5
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389516B2

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