Cyromazine → HCID 20147132, 화합물

HRID 569470

반응식

HRID 569470 반응식
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

참가 물질

5

반응물 2

HCID 47866CyromazineHCID 62365Isobutyl chloroformate

생성물 1

HCID 20147132HCID 20147132, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7b155abe100d4b31855dc61131fa66b2
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04732899

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