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Hydrochloric Acid → 2-Chloro-6-methyl-4-(tetrahydro-2H-pyran-2-yl)pyridine-3,5-dicarbonitrile

HRID 1873581
ノート
印刷プレビュー

反応式

HRID 1873581 の反応式
N[C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][O:11]2)[C:5]([C:16]#[N:17])=[C:4]([CH3:18])[N:3]=1.N(OCCC(C)C)=O.[ClH:27]>C(#N)C.[Cu](Cl)Cl>[Cl:27][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][O:11]2)[C:5]([C:16]#[N:17])=[C:4]([CH3:18])[N:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 686980092-Amino-6-methyl-4-(tetrahydro-2H-pyran-2-yl)pyridine-3,5-dicarbonitrile

生成物 1

HCID 866383962-Chloro-6-methyl-4-(tetrahydro-2H-pyran-2-yl)pyridine-3,5-dicarbonitrile

試薬・触媒・溶媒 2

HCID 24014Cupric Chloride触媒
HCID 6342
Acetonitrile
溶媒

反応条件

温度
60 °C

実験手順

610 mg (2.52 mmol) of the compound from Example 39A are initially charged in 44 ml of acetonitrile, and 590 mg (5.04 mmol) of isopentyl nitrite and 677 mg (5.04 mmol) of copper(II) chloride are added. The reaction mixture is stirred at 60° C. for 30 min. 40 ml of 1 N hydrochloric acid are then added to the mixture and the mixture is extracted three times with in each case 100 ml of ethyl acetate. The combined organic phases are dried over magnesium sulfate and the solvent is removed on a rotary evaporator. The product is used in the next reaction without further purification.

後処理

  1. extractionthe mixture is extracted three times with in each case 100 ml of ethyl acetate
  2. dry with materialThe combined organic phases are dried over magnesium sulfate
  3. customthe solvent is removed on a rotary evaporator
  4. customThe product is used in the next reaction without further purification

出典と根拠

ORDレコード
ord-6095a4f546834cb89aeaf15bbe4bea82
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304412B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート