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

HRID 372638
ノート
印刷プレビュー

反応式

HRID 372638 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile収率 51.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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°.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-35d9fab74f5c4c15b46e7358f66413e6
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04092150

反応ノート

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