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Sodium Hydroxide → 6-Chloro-2-methyl-3-(1H-1,2,3-triazol-4-yl)pyridine

HRID 385973
ノート
印刷プレビュー

反応式

HRID 385973 の反応式
C(OC[N:9]1[CH:13]=[C:12]([C:14]2[C:15]([CH3:21])=[N:16][C:17]([Cl:20])=[CH:18][CH:19]=2)[N:11]=[N:10]1)(=O)C(C)(C)C.[OH-].[Na+]>CO>[Cl:20][C:17]1[N:16]=[C:15]([CH3:21])[C:14]([C:12]2[N:11]=[N:10][NH:9][CH:13]=2)=[CH:19][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59525806[4-(6-Chloro-2-methylpyridin-3-yl)-1H-1,2,3-triazol-1-yl]methyl pivalate

生成物 1

HCID 1784328616-Chloro-2-methyl-3-(1H-1,2,3-triazol-4-yl)pyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

[4-(6-Chloro-2-methylpyridin-3-yl)-1H-1,2,3-triazol-1-yl]methyl pivalate (350 mg, 0.96 mmol) was taken up in methanol (3.9 ml) at room temperature. Aqueous sodium hydroxide (1.0M, 4.8 ml, 4.8 mmol) was added, and the mixture was allowed to react for 2 hours. The reaction was then extracted three times with diethyl ether. The combined organic fractions were washed with water. The combined aqueous layers were adjusted to pH 7.0 via dropwise addition of 6 M aqueous hydrochloric acid. The neutralized mixture was saturated with solid sodium chloride and extracted three times with ethyl acetate. All the organic layers were combined, dried over anhydrous magnesium sulfate, filtered, and concentrated to afford the title compound.

後処理

  1. customto react for 2 hours
  2. extractionThe reaction was then extracted three times with diethyl ether
  3. washThe combined organic fractions were washed with water
  4. additionThe combined aqueous layers were adjusted to pH 7.0 via dropwise addition of 6 M aqueous hydrochloric acid
  5. extractionextracted three times with ethyl acetate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-d56a19a36c594441bb69022950a35546
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367706B2

反応ノート

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