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Ammonia → HCID 13579894, 화합물

HRID 235627
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HRID 235627 반응식
[Cl:1][C:2]1[C:7]([S:8][CH3:9])=[C:6](Cl)[N:5]=[C:4]([NH:11][CH2:12][CH2:13][CH2:14][O:15][CH:16]([CH3:18])[CH3:17])[N:3]=1.[NH3:19]>CO>[NH2:19][C:6]1[C:7]([S:8][CH3:9])=[C:2]([Cl:1])[N:3]=[C:4]([NH:11][CH2:12][CH2:13][CH2:14][O:15][CH:16]([CH3:18])[CH3:17])[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 135798934,6-Dichloro-2-(3-isopropoxypropylamino)-5-methylthiopyrimidine

생성물 1

HCID 13579894HCID 13579894, 화합물수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

100 g (0.322 mole) of 4,6-dichloro-2-(3-isopropoxypropylamino)-5-methylthio-pyrimidine are dissolved in 400 ml of methanol and the solution is heated at 100° C. with 500 ml of ammonia in an autoclave for 3 hours. The undissolved residue is filtered off. After the methanol phase has been concentrated, the residue which remains is taken up in methylene chloride, the mixture is washed with water and the resulting organic phase is dried. After removal of the solvent, the resulting oil is stirred with petroleum ether. The crystals thereby obtained are filtered off with suction. 81 g (87% of theory) of the desired pyrimidine, melting point: 76° C., are obtained.

후처리

  1. filtrationThe undissolved residue is filtered off
  2. concentrationAfter the methanol phase has been concentrated
  3. washthe mixture is washed with water
  4. customthe resulting organic phase is dried
  5. customAfter removal of the solvent
  6. customThe crystals thereby obtained
  7. filtrationare filtered off with suction

출처 및 근거

ORD 기록
ord-0046d8d5c61349f4a315a2b8ae469a5a
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04640923

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