Dichloromethane → HCID 178452819, 화합물

HRID 26443

반응식

HRID 26443 반응식
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:10]2[CH2:15][CH:14]=[CH:13][CH2:12][CH2:11]2)[N:3]=1.C(Cl)Cl.[CH2:19]([O:23][C:24](Cl)=[O:25])[CH2:20][CH2:21][CH3:22]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[O:25])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 61140Butyl chloroformateHCID 178507852HCID 178507852, 화합물

생성물 1

HCID 178452819HCID 178452819, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

반응 조건

온도
5 °C

실험 절차

20 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed with 250 ml. of methylene chloride and 35 ml. of triethylamine, stirred and cooled to 5° C. The mixture is treated with 45 ml. of chloroformic acid butyl ester and stirred at room temperature for 6 hours. The mixture obtained is washed with water, extracted with methylene chloride and evaporated under reduced pressure. The residue is recrystallized from ethanol, there being obtained dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 131°-132° C.

후처리

  1. additionThe mixture is treated with 45 ml
  2. customThe mixture obtained
  3. washis washed with water
  4. extractionextracted with methylene chloride
  5. customevaporated under reduced pressure
  6. customThe residue is recrystallized from ethanol, there

출처 및 근거

ORD 기록
ord-aaf95424dd714d558075c4f775f387bd
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150132

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