Hydrochloric Acid → 4-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione

HRID 2171472

反応式

HRID 2171472 の反応式
[Na].[NH2:2][C:3]([NH2:5])=[S:4].C([O-])C.[Na+].N[C:11]([C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=1[Cl:22])=[CH:12][C:13]#[N:14].Cl>C(O)C.O>[NH2:14][C:13]1[CH:12]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=2[Cl:22])[NH:5][C:3](=[S:4])[N:2]=1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 2723790ThioureaHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 669113223-Amino-3-(2,4-dichlorophenyl)acrylonitrile

生成物 1

HCID 583059934-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

16.51 g (718.08 mmol) of sodium are dissolved in 353 ml of ethanol, and 40.996 g (538.56 mmol) of thiourea are added to the sodium ethanolate solution prepared in this way, followed by 76.5 g (359.04 mmol) of 3-amino-3-(2,4-dichlorophenyl)acrylonitrile. The mixture is heated under reflux for 18 h and, after cooling, 500 ml of water are added. The mixture is neutralized with 1M hydrochloric acid, and the precipitate which has separated out is filtered off with suction. The latter is washed with water, suspended in THF and again filtered off with suction. It is washed with 300 ml of petroleum ether and then dried under high vacuum. 67.5 g (55% of theory) of the product are obtained as a solid.

後処理

  1. customprepared in this way
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 18 h
  4. temperatureafter cooling
  5. customthe precipitate which has separated out
  6. filtrationis filtered off with suction
  7. washThe latter is washed with water
  8. filtrationagain filtered off with suction
  9. washIt is washed with 300 ml of petroleum ether
  10. customdried under high vacuum
  11. custom67.5 g (55% of theory) of the product are obtained as a solid

出典と根拠

ORDレコード
ord-7388652bd41144639ea28a102170f284
出典データセット
uspto-grants-2015_06
特許番号
US09051323B2

関連ノート

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