Water → 6-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine

HRID 2389734

反応式

HRID 2389734 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[Cl:15])[NH:5][C:4](=[S:16])[N:3]=1.I[CH2:18][CH3:19].C(=O)(O)[O-].[Na+].O>CS(C)=O>[Cl:15][C:9]1[CH:10]=[C:11]([Cl:14])[CH:12]=[CH:13][C:8]=1[C:6]1[N:5]=[C:4]([S:16][CH2:18][CH3:19])[N:3]=[C:2]([NH2:1])[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 516892Sodium BicarbonateHCID 583059934-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione

生成物 1

HCID 583060056-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

67.5 g (248 mmol) of 4-amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione and 77.37 g (496.04 mmol) of iodoethane are dissolved in 560 ml of dry DMSO and, at RT, 270 ml of a saturated aqueous sodium bicarbonate solution are slowly added. The mixture is stirred at RT for 5 h and then 440 ml of water are added. The precipitate is filtered off with suction, washed with water and sucked dry. It is stirred twice with 100 ml of isopropanol each time and again filtered off with suction. It is washed once more with petroleum ether and the residue is dried under high vacuum. 50.0 g (67% of theory) of the product are obtained as a solid.

後処理

  1. filtrationThe precipitate is filtered off with suction
  2. washwashed with water
  3. customsucked dry
  4. stirringIt is stirred twice with 100 ml of isopropanol each time
  5. filtrationagain filtered off with suction
  6. washIt is washed once more with petroleum ether
  7. customthe residue is dried under high vacuum
  8. custom50.0 g (67% of theory) of the product are obtained as a solid

出典と根拠

ORDレコード
ord-b36d2978298b4e7a9f7c9425e1fc4cc1
出典データセット
uspto-grants-2012_09
特許番号
US08273752B2

関連ノート

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