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Sodium Carbonate → 4-Chloro-6-methyl-2-(6-n-propyl-2-pyridinyl)pyrimidine

HRID 580322
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HRID 580322 반응식
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH3:17])[N:10]=2)[N:3]=1.P(Cl)(Cl)([Cl:20])=O.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1>[Cl:20][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH3:17])[N:10]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 178438999HCID 178438999, 화합물

생성물 1

HCID 142532544-Chloro-6-methyl-2-(6-n-propyl-2-pyridinyl)pyrimidine수율 93.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To solution of 4-hydroxy-6-methyl-2-(6-n-propyl-2-pyridinyl)pyrimidine (2 g) in toluene (20 ml), was added phosphoryl chloride (2 g). The mixture was heated under refluxing for one hour and left to stand to room temperature. Aqueous sodium carbonate solution was added thereto until the reaction solution became about pH 8 to be separated into two layers. Toluene layer was collected and washed with water and dried over anhydrous magnesium sulfate. The toluene layer was concentrated under reduced pressure to obtain 4-chloro-6-methyl-2-(6-n-propyl-2-pyridinyl)pyrimidine (2.03 g).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder refluxing for one hour
  3. waitleft
  4. customto stand to room temperature
  5. customto be separated into two layers
  6. customToluene layer was collected
  7. washwashed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationThe toluene layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ba9259d5a13e4010b2a2acdfb0169958
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04752608

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