Formaldehyde → 4,6-Dimethyl-2-(morpholin-4-ylthiocarbonylthiomethylamino)pyrimidine

HRID 34865

反応式

HRID 34865 の反応式
[OH-].[K+].[NH:3]1[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1.[C:9](=[S:11])=[S:10].C=O.[NH2:14][C:15]1[N:20]=[C:19]([CH3:21])[CH:18]=[C:17]([CH3:22])[N:16]=1.[CH3:23]S(O)(=O)=O>O>[CH3:22][C:17]1[CH:18]=[C:19]([CH3:21])[N:20]=[C:15]([NH:14][CH2:23][S:10][C:9]([N:3]2[CH2:8][CH2:7][O:6][CH2:5][CH2:4]2)=[S:11])[N:16]=1

参加物

8

反応物 6

HCID 712FormaldehydeHCID 6348Carbon DisulfideHCID 6395Methanesulfonic AcidHCID 8083MorpholineHCID 130212-Amino-4,6-dimethyl pyrimidineHCID 14797Potassium Hydroxide

生成物 1

HCID 539986464,6-Dimethyl-2-(morpholin-4-ylthiocarbonylthiomethylamino)pyrimidine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

6.6 g (0.1 mole) of 85% potassium hydroxide and 8.9 g (0.1 mole) of morpholine are dissolved in 200 ml of water and, with cooling, 7.7 g (0.1 mole) of carbon disulfide are added. The mixture is stirred until a yellowish homogeneous solution is obtained. With cooling and stirring, 9.4 g (0.11 mole) of aqueous 35% formaldehyde and a solution of 12.7 g (0.1 mole) of 2-amino-4,6-dimethylpyrimidine and 9.7 g (0.1 mole) of methanesulfonic acid in 50 ml of water are added in succession. The reaction mixture is further stirred at room temperature, whereupon first an oil precipitates, which crystallises after a short time. After 24 hours the batch is diluted with 1 liter of water and the crystalline precipitate is filtered with suction and dried, affording 24 g (80% of theory) of the title compound with a melting point of 119°-121° C.

後処理

  1. temperaturewith cooling
  2. customis obtained
  3. temperatureWith cooling
  4. stirringstirring
  5. stirringThe reaction mixture is further stirred at room temperature
  6. customwhereupon first an oil precipitates
  7. customwhich crystallises after a short time
  8. additionAfter 24 hours the batch is diluted with 1 liter of water
  9. filtrationthe crystalline precipitate is filtered with suction
  10. customdried

出典と根拠

ORDレコード
ord-93a2ffbdfc7f40559b8be705008d4d29
出典データセット
uspto-grants-1988_08
特許番号
US04764203

関連ノート

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