Sulfuric Acid → HCID 86689231, 화합물

HRID 871020노트

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HRID 871020 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[CH:8]=2)[C:3]=1[C:16]#[N:17].[OH:18]S(O)(=O)=O>>[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[CH:8]=2)[C:3]=1[C:16]([NH2:17])=[O:18]

참가 물질

3

반응물 2

HCID 1118Sulfuric Acid2회HCID 86689232HCID 86689232, 화합물

생성물 1

HCID 86689231HCID 86689231, 화합물수율 86%

반응 조건

온도
65 °C

실험 절차

A mixture of 5-amino-3-(3-nitrophenyl)isothiazole-4-carbonitrile (500 mg, 2.03 mmol) in 5 mL conc. H2SO4 was heated at 65° C. After 4 hours the mixture was slowly added to 75 mL ice water (including an additional reaction run on 0.50 mmol scale in 1.5 mL conc. H2SO4). The mixture was stirred for 10 min, and then the precipitate filtered and rinsed with water and 10% EtOAc/hexane to give the title compound as a light beige solid (572 mg, 86% combined yield).

후처리

  1. filtrationthe precipitate filtered
  2. washrinsed with water and 10% EtOAc/hexane

출처 및 근거

ORD 기록
ord-e724859f78244f11bf99c2904ee690cd
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969583B2

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