Lawesson's reagent → 2-Amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]-pyrimidin-7(8H)-thion

HRID 3173

반응식

HRID 3173 반응식
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9](=O)[N:8]([CH3:21])[C:6]=2[N:7]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:31])=CC=1>N1C=CC=CC=1>[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9](=[S:31])[N:8]([CH3:21])[C:6]=2[N:7]=1

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 53278642-amino-6-(2,6-dichlorophenyl)-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 116529512-Amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]-pyrimidin-7(8H)-thion

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 0.321 g (1.0 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7-(8H)-one from Example 12 and 0.404 g (1.0 mmol) of Lawesson's Reagent in 10 mL of pyridine was heated at reflux with stirring for 24 hours. The solvent was evaporated under reduced pressure, and the residue was triturated with 20 mL of water, filtered, and the cake washed well with water. Purification was by silica gel chromatography to afford the desired compound identified as 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]-pyrimidin-7(8H)-thione.

후처리

  1. temperaturewas heated
  2. temperatureat reflux
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was triturated with 20 mL of water
  5. filtrationfiltered
  6. washthe cake washed well with water
  7. customPurification

출처 및 근거

ORD 기록
ord-9cc63b0f6a514bce8d35b9f03404b410
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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