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Ethylamine → 4-Chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

HRID 1757894
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HRID 1757894 반응식
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[N:5]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:3]=1.[CH2:15]([NH2:17])[CH3:16]>CC(C)=O>[Cl:10][C:6]1[C:7]([C:8]#[N:9])=[C:2]([NH:17][CH2:15][CH3:16])[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:5]=1
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참가 물질

4

반응물 2

HCID 6341EthylamineHCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile

생성물 1

HCID 205102154-Chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A stirred solution of 3.5 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile in 100 ml of acetone was cooled to between 0° and -5°; a solution of 2.1 grams of aqueous 70% ethylamine in 25 ml of acetone was added dropwise. Upon complete addition, the reaction mixture was warmed to room temperature and stirred for 18 hours. The acetone was removed under reduced pressure, and the residue was extracted with a mixture of diethyl ether and water. The organic layer was separated and dried over magnesium sulfate. The mixture was filtered, and the filtrate was evaporated to dryness under reduced pressure. The residue was recrystallized from methylcyclohexane to give 3.1 grams of 4-chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 144°-146°.

후처리

  1. additionUpon complete addition
  2. customThe acetone was removed under reduced pressure
  3. extractionthe residue was extracted with a mixture of diethyl ether and water
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe mixture was filtered
  7. customthe filtrate was evaporated to dryness under reduced pressure
  8. customThe residue was recrystallized from methylcyclohexane

출처 및 근거

ORD 기록
ord-bad01174da774ef2a6e8e11419cb7b77
출처 데이터셋
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE031136

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