Ethanol → HCID 178527812、化合物

HRID 48295ノート

反応式

HRID 48295 の反応式
CC(C)CN[C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[CH:7][C:6]=1[NH2:15].[C:17](=[S:19])=[S:18].C(O)C>[OH-].[Na+]>[S:18]1[C:5]2[C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[N:8]=[CH:7][C:6]=2[N:15]=[C:17]1[SH:19]

参加物

5

反応物 3

HCID 702EthanolHCID 6348Carbon DisulfideHCID 11298872N4-(2-methylpropyl)quinoline-3,4-diamine

生成物 1

HCID 178527812HCID 178527812、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

N4-(2-methylpropyl)quinoline-3,4-diamine (5.4 g, 25 mmol) was combined with carbon disulfide (9 mL, 150 mmol) and ethanol (55 mL) and then heated at reflux on a steam bath for 2 hours. The resulting precipitate was isolated by filtration, washed with ethanol and then air dried to provide 4.4 g of crude product. A portion (1 g) was dissolved in hot dilute sodium hydroxide and then reprecipitated with acetic acid. The precipitate was isolated by filtration while still hot, washed with hexane and then air dried to provide thiazolo[4,5-c]quinoline-2-thiol as a solid, m.p. 282-284° C. Analysis: Calculated for C10H6N2S2: %C, 55.02; %H, 2.77; %N, 12.83: Found: %C, 54.96; %H, 2.69; %N, 12.74.

後処理

  1. temperatureheated
  2. temperatureat reflux on a steam bath for 2 hours
  3. customThe resulting precipitate was isolated by filtration
  4. washwashed with ethanol
  5. customair dried
  6. customto provide 4.4 g of crude product
  7. customreprecipitated with acetic acid
  8. customThe precipitate was isolated by filtration while still hot,
  9. washwashed with hexane
  10. customair dried

出典と根拠

ORDレコード
ord-bf8a366e53444547b50e58f7ba7ad65d
出典データセット
uspto-grants-2004_03
特許番号
US06703402B2

反応ノート

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