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Sodium → 2-Amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine

HRID 3909
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HRID 3909 반응식
[NH2:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([CH:9]=[C:10]([Cl:12])[Cl:11])[N:3]=1.[CH3:13][O-:14].[Na+].[Na]>CO>[NH2:1][C:2]1[N:3]=[C:4]([CH:9]=[C:10]([Cl:12])[Cl:11])[CH:5]=[C:6]([O:14][CH3:13])[N:7]=1
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참가 물질

5

반응물 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 201535042-Amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine

생성물 1

HCID 201535032-Amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

22.0 Parts of 2-amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine was dissolved in 500 parts of dry methanol and stirred whilst a solution of sodium methoxide, prepared by dissolving 4.6 parts of sodium in 200 parts of dry methanol, was added dropwise, over 30 minutes at ambient temperature. The resulting solution was stirred for 4 hours by which time all the starting material had been consumed. The product was precipitated by the addition of water, filtered and dried. The solid obtained was purified by chromatography on silica using diethyl ether as eluent. Final purification was effected by recrystallisation from carbon tetrachloride to give 2-amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine m.p. 90°-91° C.

후처리

  1. customprepared
  2. additionwas added dropwise, over 30 minutes at ambient temperature
  3. customhad been consumed
  4. customThe product was precipitated by the addition of water
  5. filtrationfiltered
  6. customdried
  7. customThe solid obtained
  8. customwas purified by chromatography on silica
  9. customFinal purification
  10. customwas effected by recrystallisation from carbon tetrachloride

출처 및 근거

ORD 기록
ord-c486bd8087ef4bc39cbd7955c7ea7c4c
출처 데이터셋
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04723006

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