Cyromazine → HCID 20147132、化合物

HRID 569470

反応式

HRID 569470 の反応式
Cl[C:2]([O:4][CH2:5][CH:6]([CH3:8])[CH3:7])=[O:3].[NH2:9][C:10]1[N:15]=[C:14]([NH2:16])[N:13]=[C:12]([NH:17][CH:18]2[CH2:20][CH2:19]2)[N:11]=1>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[CH:18]1([NH:17][C:12]2[N:11]=[C:10]([NH:9][C:2]([O:4][CH2:5][CH:6]([CH3:8])[CH3:7])=[O:3])[N:15]=[C:14]([NH:16][C:2]([O:4][CH2:5][CH:6]([CH3:8])[CH3:7])=[O:3])[N:13]=2)[CH2:20][CH2:19]1

参加物

5

反応物 2

HCID 47866CyromazineHCID 62365Isobutyl chloroformate

生成物 1

HCID 20147132HCID 20147132、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

16.4 g (0.12 mol) of isobutyl chloroformate are added dropwise to a mixture of 8.3 g (0.05 mol) of 2,4-diamino-6-cyclopropylamino-s-triazine, 0.5 g of 4-dimethylaminopyridine and 125 ml of pyridine. The batch is stirred for 1 hour at room temperature and then for 1 hour at 55°-60° C. After the precipitate has been filtered off, the reaction mixture is concentrated by evaporation in a water-jet vacuum, the residue is taken up in 150 ml of chloroform and extracted with 100 ml of water. After drying over sodium sulfate, the solvent is distilled off, and the crude product is purified by column chromatography through silica with methylene chloride as eluant.

後処理

  1. waitfor 1 hour at 55°-60° C
  2. filtrationAfter the precipitate has been filtered off
  3. concentrationthe reaction mixture is concentrated by evaporation in a water-jet vacuum
  4. extractionextracted with 100 ml of water
  5. dry with materialAfter drying over sodium sulfate
  6. distillationthe solvent is distilled off
  7. customthe crude product is purified by column chromatography through silica with methylene chloride as eluant

出典と根拠

ORDレコード
ord-7b155abe100d4b31855dc61131fa66b2
出典データセット
uspto-grants-1988_03
特許番号
US04732899

関連ノート

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