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Hydrogen Peroxide → (1S,2S,5R)-2-isopropyl-5-methylcyclohexanecarboxamide

HRID 407530
ノート
印刷プレビュー

反応式

HRID 407530 の反応式
[CH:1]([C@@H:4]1[CH2:9][CH2:8][C@@H:7]([CH3:10])[CH2:6][C@@H:5]1[C:11]#[N:12])([CH3:3])[CH3:2].[OH:13]O.[OH-].[Na+]>CS(C)=O.O>[CH:1]([C@@H:4]1[CH2:9][CH2:8][C@@H:7]([CH3:10])[CH2:6][C@@H:5]1[C:11]([NH2:12])=[O:13])([CH3:3])[CH3:2]
参加物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 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 11073771(1S,2S,5R)-Neomenthyl cyanide

生成物 1

HCID 59253418(1S,2S,5R)-2-isopropyl-5-methylcyclohexanecarboxamide

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

A solution of 0.105 g (0.634 mmol) of (1S,2S,5R)-2-isopropyl-5-methylcyclohexanecarbonitrile in 4.9 mL of dimethyl sulfoxide was placed in a 10 mL flask with a magnetic stir bar. After adding 0.60 mL of 35% hydrogen peroxide and 0.097 g (1.2 mmol) of 50% sodium hydroxide solutions the flask was capped and stirred at room temperature for 20 h. The reaction mixture was diluted with 10 mL of water, extracted twice with 10 mL of methylene chloride. The combined methylene chloride layers were back extracted with 3×20 mL of water, dried over magnesium sulfate, and concentrated in vacuo to provide an off-white solid that was further purified by column chromatography (silica gel, 75:25 hexane:ethyl acetate) to provide (1S,2S,5R)-2-isopropyl-5-methylcyclohexanecarboxamide.

後処理

  1. customwas capped
  2. extractionextracted twice with 10 mL of methylene chloride
  3. extractionThe combined methylene chloride layers were back extracted with 3×20 mL of water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customto provide an off-white solid
  7. customthat was further purified by column chromatography (silica gel, 75:25 hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-a97f5bb11f954bae87492f963bccf1c9
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08754259B2

反応ノート

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