Stannous chloride dihydrate → HCID 136388576、化合物

HRID 131379

反応式

HRID 131379 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[S:10][CH:11]=[CH:12][C:13]=2[C:14]#[N:15])=[C:4]([N+:16]([O-])=O)[CH:3]=1.O.O.[Sn](Cl)Cl>C(O)C.Cl>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:9]3[S:10][CH:11]=[CH:12][C:13]=3[C:14]([NH2:15])=[N:16][C:4]=2[CH:3]=1

参加物

5

反応物 2

HCID 61436Stannous chloride dihydrateHCID 692103022-(4-Chloro-2-nitro-phenylamino)-thiophene-3-carbonitrile

生成物 1

HCID 136388576HCID 136388576、化合物収率 142.2%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

Suspend 2-(4-chloro-2-nitro-phenylamino)-thiophene-3-carbonitrile (4.85 g, 17.35 mmol) in ethanol (40.0 ml). Dissolve tin(II) chloride dihydrate (11.75 g, 52.06 mmol) in 5N HCl (40.0 ml) and then add it to the suspension. Heat the reaction at reflux for 48 hours. Cool the reaction to ambient temperature and then chill it in a refrigerator for 2 hours. Collect the resulting precipitate by vacuum filtration and then dry it under vacuum to give 3.53 g (71%) of the title compound: mass spectrum (ion spray): m/z=250.0 (M+1).

後処理

  1. temperatureHeat
  2. customthe reaction
  3. temperatureat reflux for 48 hours
  4. temperatureCool
  5. customthe reaction to ambient temperature
  6. temperaturechill it in a refrigerator for 2 hours
  7. customCollect the resulting precipitate
  8. filtrationby vacuum filtration
  9. customdry it under vacuum

出典と根拠

ORDレコード
ord-623c2cee87cf4f29af7e5b80f35fc012
出典データセット
uspto-grants-2008_06
特許番号
US07384934B2

関連ノート

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