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Hydrochloric Acid → 2-Chloro-6-{[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methoxy}-4-[4-(2-hydroxyethoxy)phenyl]-pyridine-3,5-dicarbonitrile

HRID 1913504
ノート
印刷プレビュー

反応式

HRID 1913504 の反応式
N(OCCC(C)C)=O.N[C:10]1[C:15]([C:16]#[N:17])=[C:14]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][OH:27])=[CH:20][CH:19]=2)[C:13]([C:28]#[N:29])=[C:12]([O:30][CH2:31][C:32]2[N:33]=[C:34]([C:37]3[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=3)[O:35][CH:36]=2)[N:11]=1.[ClH:44]>C(#N)C.[Cu](Cl)Cl>[Cl:44][C:10]1[C:15]([C:16]#[N:17])=[C:14]([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][OH:27])=[CH:22][CH:23]=2)[C:13]([C:28]#[N:29])=[C:12]([O:30][CH2:31][C:32]2[N:33]=[C:34]([C:37]3[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=3)[O:35][CH:36]=2)[N:11]=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 666721372-Amino-6-{[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methoxy}-4-[4-(2-hydroxyethoxy)phenyl]pyridine-3,5-dicarbonitrile

生成物 1

HCID 866496412-Chloro-6-{[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methoxy}-4-[4-(2-hydroxyethoxy)phenyl]-pyridine-3,5-dicarbonitrile

試薬・触媒・溶媒 2

HCID 24014
Cupric Chloride
触媒
HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

78 mg (0.67 mmol) of isopentyl nitrite and 90 mg (0.67 mmol) of copper(II) chloride were initially charged in 8.5 ml of acetonitrile, and 72 mg (0.64 mmol) of the compound from Example 49A were added. The reaction mixture was stirred at 60° C. for 3 h. 8.5 ml of 1N hydrochloric acid were added to the reaction solution. The aqueous phase was extracted twice with in each case 20 ml of ethyl acetate, and the combined organic phases were dried over magnesium sulfate. After removal of the solvent on a rotary evaporator, the residue was dried under reduced pressure and used without further purification for the subsequent reaction.

後処理

  1. extractionThe aqueous phase was extracted twice with in each case 20 ml of ethyl acetate
  2. dry with materialthe combined organic phases were dried over magnesium sulfate
  3. customAfter removal of the solvent
  4. customon a rotary evaporator
  5. customthe residue was dried under reduced pressure
  6. customused without further purification for the subsequent reaction

出典と根拠

ORDレコード
ord-3632816299e44feab97006dcef0a7cfe
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609686B2

反応ノート

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