Ethylamine → 2-Ethylamino-4,6-dichloro-5-methylthio-pyrimidine

HRID 1862827노트

반응식

HRID 1862827 반응식
Cl[C:2]1[N:7]=[C:6]([Cl:8])[C:5]([S:9][CH3:10])=[C:4]([Cl:11])[N:3]=1.[CH2:12]([NH2:14])[CH3:13].[OH-].[Na+]>CC(CC)=O>[CH2:12]([NH:14][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([S:9][CH3:10])=[C:4]([Cl:11])[N:3]=1)[CH3:13]

참가 물질

5

반응물 3

HCID 6341EthylamineHCID 14798Sodium HydroxideHCID 122255442,4,6-Trichloro-5-methylsulfanyl-pyrimidine

생성물 1

HCID 155677722-Ethylamino-4,6-dichloro-5-methylthio-pyrimidine

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

230 parts of 2,4,6-trichloro-5-methylthio-pyrimidine are dissolved in 740 parts of methylethylketone, 650 parts of ice are added, and 120 parts of an aqueous 38% solution of ethylamine are run in over 30 minutes while cooling in order that the temperature should not exceed 5° C. 129.5 parts of a 31% solution of caustic soda are added in a period of an hour at 20° C. and the mixture is stirred for 6 hours. The desired isomer is then precipitated while the 4-ethylamino-2,6-dichloro-5-methylthiopyrimidine remains in solution. After cooling for 15 hours, the product is filtered off and washed with methylethylketone. 73 parts of the desired product are obtained, which is recrystallised from ethanol. M.p. 147° C.

후처리

  1. additionare added
  2. customare run in over 30 minutes
  3. temperaturewhile cooling in order that the temperature should not
  4. customexceed 5° C
  5. customThe desired isomer is then precipitated while the 4-ethylamino-2,6-dichloro-5-methylthiopyrimidine
  6. temperatureAfter cooling for 15 hours
  7. filtrationthe product is filtered off
  8. washwashed with methylethylketone

출처 및 근거

ORD 기록
ord-a7b367d959954635bed937cde5b74a05
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04166852

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