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

HRID 2171473

반응식

HRID 2171473 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00ccfb01c6544563b70b06cf24c6caf1
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051323B2

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