Diethylamine → 4-Chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

HRID 372644노트

반응식

HRID 372644 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]([NH:17][CH2:18][CH3:19])[CH3:16]>C(OCC)C>[Cl:10][C:6]1[C:7]([C:8]#[N:9])=[C:2]([N:17]([CH2:18][CH3:19])[CH2:15][CH3:16])[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:5]=1

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile

생성물 1

HCID 205102144-Chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile수율 50.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a stirred solution of 4.3 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile in 125 ml of diethyl ether was added dropwise 2.6 grams of diethylamine. Upon complete addition, the reaction mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed with water. The diethyl ether layer was separated and dried over magnesium sufate. The mixture was filtered, and the filtrate was evaporated under reduced pressure to a residue. The residue was recrystallized from methylcyclohexane to give 2.5 grams of 4-chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 74°-76°.

후처리

  1. additionUpon complete addition
  2. washThe reaction mixture was washed with water
  3. customThe diethyl ether layer was separated
  4. dry with materialdried over magnesium sufate
  5. filtrationThe mixture was filtered
  6. customthe filtrate was evaporated under reduced pressure to a residue
  7. customThe residue was recrystallized from methylcyclohexane

출처 및 근거

ORD 기록
ord-15002aec74e3494a94c97b14db23f6ca
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04092150

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