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Water → 4,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile

HRID 372638
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HRID 372638 반응식
Cl[C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]#[N:10])=[C:4]([Cl:11])[N:3]=1.[CH:12]([NH2:15])([CH3:14])[CH3:13].O>C(OCC)C>[Cl:11][C:4]1[C:5]([C:9]#[N:10])=[C:6]([Cl:8])[N:7]=[C:2]([NH:15][CH:12]([CH3:14])[CH3:13])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6363IsopropylamineHCID 2509452,4,6-Trichloro-5-cyanopyrimidine

생성물 1

HCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile수율 51.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A stirred solution of 4.2 grams of 2,4,6-trichloro-5-pyrimidinecarbonitrile in 100 ml of diethyl ether was cooled to between -5° and -10°, and a solution of 2.4 grams of isopropylamine in 100 ml of diethyl ether was added dropwise. Upon complete addition, water was added to the reaction mixture, and the ether layer was separated. The ethereal layer was dried over magnesium sulfate and filtered. The filtrate was evaporated to dryness under reduced pressure. The residue was recrystallized from methylcyclohexane to give 2.4 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 179°-181°.

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후처리

  1. additionwas added to the reaction mixture
  2. customthe ether layer was separated
  3. dry with materialThe ethereal layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness under reduced pressure
  6. customThe residue was recrystallized from methylcyclohexane

출처 및 근거

ORD 기록
ord-35d9fab74f5c4c15b46e7358f66413e6
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04092150

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