Sulfuric Acid → HCID 86689231、化合物

HRID 871020ノート

反応式

HRID 871020 の反応式
[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]

参加物

3

反応物 2

HCID 1118Sulfuric Acid2 回HCID 86689232HCID 86689232、化合物

生成物 1

HCID 86689231HCID 86689231、化合物収率 86%

反応条件

温度
65 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e724859f78244f11bf99c2904ee690cd
出典データセット
uspto-grants-2015_03
特許番号
US08969583B2

反応ノート

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