Cyanuric chloride → 4,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine

HRID 325969

반응식

HRID 325969 반응식
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].C(=O)(O)[O-].[Na+].Cl.[CH2:16]([O:18][C:19](=[O:22])[CH2:20][NH2:21])[CH3:17]>CC(C)=O>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([NH:21][CH2:20][C:19]([O:18][CH2:16][CH3:17])=[O:22])[N:7]=1

참가 물질

5

반응물 3

HCID 7954Cyanuric chlorideHCID 516892Sodium BicarbonateHCID 2723640Glycine ethyl ester, hydrochloride

생성물 1

HCID 147462614,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine수율 51.9%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 10 g of ice water was added 1.84 g of cyanuric chloride dissolved in 50 ml of acetone. To this solution kept at an internal temperature of 0° to 5° C. under stirring were added 1.68 g of sodium bicarbonate and 1.40 g of glycine ethylester hydrochloride and the mixture was stirred at said temperature for 30 minutes. The reaction product was extracted with ethyl acetate and dried with sodium sulfate. Then, ethyl acetate was distilled out and separated crystal was recrystallized from cyclohexane to obtain 1.3 g of 4,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine which had a melting point of 89° to 90.5° C.

후처리

  1. customkept at an internal temperature of 0° to 5° C.
  2. stirringthe mixture was stirred
  3. customfor 30 minutes
  4. extractionThe reaction product was extracted with ethyl acetate
  5. dry with materialdried with sodium sulfate
  6. distillationThen, ethyl acetate was distilled out
  7. customseparated crystal
  8. customwas recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-6eb8874b925d4cb5a681e519d504615f
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04443531

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