Triethylamine → 6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Dimethylthiocarbamate

HRID 66719ノート

反応式

HRID 66719 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]([Cl:12])([Cl:11])[Cl:10])[N:3]=1.C(N(CC)CC)C.[CH3:20][N:21]([CH3:25])[C:22](Cl)=[S:23]>CCOCC>[CH3:20][N:21]([CH3:25])[C:22](=[S:23])[O:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]([Cl:12])([Cl:10])[Cl:11])[N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27871Dimethylthiocarbamoyl chlorideHCID 178429333HCID 178429333、化合物

生成物 1

HCID 130415306-Methyl-2-Trichloromethyl-4-Pyrimidinyl Dimethylthiocarbamate収率 55%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.6 g (0.025 mole) triethylamine, 3.2 g (0.025 mole) dimethylthiocarbamoyl chloride, and 100 ml ether was refluxed 16 hours. A trace of dark solid was filtered out and the solution was evaporated on a steam bath to give a solid residue. This residue was extracted with hot ligroin to yield 4.3 g (55% yield) of product (mp 81°-83° C.) on cooling. The structure was confirmed via infrared and elemental analysis.

後処理

  1. temperaturewas refluxed 16 hours
  2. filtrationA trace of dark solid was filtered out
  3. customthe solution was evaporated on a steam bath
  4. customto give a solid residue
  5. extractionThis residue was extracted with hot ligroin

出典と根拠

ORDレコード
ord-61635044421b488eb86f93ade7559371
出典データセット
uspto-grants-1982_08
特許番号
US04343803

反応ノート

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