1,2,3,6-Tetrahydropyridine → 2-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate

HRID 27232

반응식

HRID 27232 반응식
[NH2:1][C:2]1[N+:7]([O-])=[C:6]([NH:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])[CH:5]=[C:4](Cl)[N:3]=1.[NH:18]1[CH2:23][CH2:22][CH:21]=[CH:20][CH2:19]1>C(Cl)(Cl)Cl>[NH2:1][C:2]1[N:7]=[C:6]([NH:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])[CH:5]=[C:4]([N:18]2[CH2:19][CH:20]=[CH:21][CH2:22][CH2:23]2)[N:3]=1

참가 물질

4

반응물 2

HCID 127501,2,3,6-TetrahydropyridineHCID 178496340HCID 178496340, 화합물

생성물 1

HCID 202857752-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
45 °C

실험 절차

2.5 G. of 2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide are mixed under argon with 3 ml. of 1,2,5,6-tetrahydropyridine and 25 ml. of chloroform. The mixture is stirred at 45° C. for 12 hours, then cooled and washed with 15 ml. of water. The product is extracted with chloroform, the organic phase is dried over sodium sulfate and the solvent is distilled off under reduced pressure. The residue obtained is crystallized from methylene chloride/ether, there being obtained pure 2-methoxyethyl 2-amino-6-[3,6-dihydro-1(2H)-pyridyl]-4-pyrimidinecarbamate having a melting point of 136° C.

후처리

  1. temperaturecooled
  2. washwashed with 15 ml
  3. extractionThe product is extracted with chloroform
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue obtained
  7. customis crystallized from methylene chloride/ether, there

출처 및 근거

ORD 기록
ord-0b729c248c43465bb70369dea04a29fa
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220772

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