m-Chloroperbenzoic acid → HCID 12094929、化合物

HRID 1767762ノート

反応式

HRID 1767762 の反応式
[C:1]1([C:6]2[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=2)[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:5][CH2:4][CH2:3][CH:2]=1.ClC1C=CC=C(C(OO)=[O:25])C=1>C(Cl)Cl>[C:1]12([C:6]3[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=3)[C:9]([O:11][CH2:12][CH3:13])=[O:10])[O:25][CH:5]1[CH2:4][CH2:3][CH2:2]2

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 12094926Ethyl 3-cyclopenten-1-ylbenzoate

生成物 1

HCID 12094929HCID 12094929、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

5 g (23 mmol) of ethyl 3-cyclopent-1-ylbenzoate (4a) and 100 ml of methylene chloride are introduced into a round-bottomed flask. The solution is cooled to 0° C. and 9 g (28 mmol) of meta-chloroperbenzoic acid are added in portions. The mixture is stirred for 30 minutes at 0° C. and then for 4 hours at room temperature. The mixture is filtered. The filtrate is successively washed with a saturated aqueous sodium thiosulfate solution, a saturated aqueous sodium bicarbonate solution and then with a saturated aqueous sodium chloride solution. The organic phase is dried over Na2SO4, filtered and concentrated under reduced pressure. The residue is purified by flash chromatography on silica gel (cyclohexane/ethyl acetate: 95:5). The title product is obtained in the form of a colorless oil (4.8 g).

後処理

  1. waitfor 4 hours at room temperature
  2. filtrationThe mixture is filtered
  3. washThe filtrate is successively washed with a saturated aqueous sodium thiosulfate solution
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue is purified by flash chromatography on silica gel (cyclohexane/ethyl acetate: 95:5)

出典と根拠

ORDレコード
ord-c5e91866ff564ecfb87353f6b6e11f99
出典データセット
uspto-grants-2007_06
特許番号
US07235568B2

反応ノート

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