m-Chloroperbenzoic acid → Methyl 2-(8,9-epoxynonyloxy)-2-methylpropionate

HRID 1796355ノート

反応式

HRID 1796355 の反応式
[CH3:1][C:2]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH:16]=[CH2:17])([CH3:7])[C:3]([O:5][CH3:6])=[O:4].ClC1C=CC=C(C(OO)=[O:26])C=1>C(Cl)Cl>[O:26]1[CH2:17][CH:16]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][O:8][C:2]([CH3:1])([CH3:7])[C:3]([O:5][CH3:6])=[O:4]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 21866680Methyl 2-methyl-2-(8-nonenyloxy)propionate

生成物 1

HCID 21866634Methyl 2-(8,9-epoxynonyloxy)-2-methylpropionate収率 101.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methyl 2-methyl-2-(8-nonenyloxy)propionate (40 g) was dissolved in 320 ml of methylene chloride, and 40.8 g of 70% 3-chloroperbenzoic acid was added with stirring under ice-cooling, and the mixture was stirred for 15 hours at room temperature. The reaction solution was filtrated to remove insolubles, and the filtrate was concentrated. The residue was dissolved in n-hexane and washed 4 times with aqueous 10% potassium carbonate solution, washed with water, dried over anhydrous magnesium sulfate and concentrated to give 43.2 g of the objective compound as colorless oil.

後処理

  1. temperaturecooling
  2. stirringthe mixture was stirred for 15 hours at room temperature
  3. filtrationThe reaction solution was filtrated
  4. customto remove insolubles
  5. concentrationthe filtrate was concentrated
  6. dissolutionThe residue was dissolved in n-hexane
  7. washwashed 4 times with aqueous 10% potassium carbonate solution
  8. washwashed with water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-25b88fd6ff9b4a74adac22c58f0af3a8
出典データセット
uspto-grants-2006_04
特許番号
US07030143B2

反応ノート

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