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Potassium Iodide → Ethyl 2-[4-(acetyloxy)-2-methylphenoxy]-2-methylpropanoate

HRID 9627
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HRID 9627 반응식
C([C:4]1[CH:18]=[CH:17][C:7]([O:8][C:9]([CH3:16])([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:6]([CH3:19])[CH:5]=1)(=O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.ClC1C=CC=[C:34]([C:38]([O:40]O)=[O:39])C=1.[I-].[K+]>ClCCl>[C:38]([O:40][C:4]1[CH:18]=[CH:17][C:7]([O:8][C:9]([CH3:15])([CH3:16])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:6]([CH3:19])[CH:5]=1)(=[O:39])[CH3:34]
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참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 6101p-Toluenesulfonic acidHCID 70297m-Chloroperbenzoic acidHCID 16756777Ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate2회

생성물 1

HCID 21986549Ethyl 2-[4-(acetyloxy)-2-methylphenoxy]-2-methylpropanoate

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

반응 조건

온도
40 °C

실험 절차

A solution of ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate (intermediate 8, 37.33 g) in dichloromethane (650 ml) was treated with 4-toluenesulphonic acid (2.75 g) followed by m-chloroperbenzoic acid (60.5 g) and the mixture warmed to 40° C. and stirred under nitrogen for 19 hours. The cooled mixture was treated with dichloromethane (350 ml) and the resulting mixture added to aqueous potassium iodide (1000 ml, 10% solution). The organic layer was collected and washed twice with water and brine, then dried over sodium sulfate, filtered and the filtrate concentrated to give the title compound as an orange oil.

후처리

  1. customThe organic layer was collected
  2. washwashed twice with water and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated

출처 및 근거

ORD 기록
ord-ac4f6997785540cfabd1e40607d0df66
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091237B2

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