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m-Chloroperbenzoic acid → (2-Ethyl-1,7,10-trioxaspiro[4.6]undecan-2-yl)methanol

HRID 647745
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HRID 647745 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]=[C:13]([CH2:24][CH3:25])[CH2:14][CH2:15][C:16]1([OH:23])[CH2:22][O:21][CH2:20][CH2:19][O:18][CH2:17]1>C(Cl)Cl>[CH2:24]([C:13]1([CH2:12][OH:9])[CH2:14][CH2:15][C:16]2([CH2:17][O:18][CH2:19][CH2:20][O:21][CH2:22]2)[O:23]1)[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 132371746-(3-Methylidenepentyl)-1,4-dioxepan-6-ol

생성물 1

HCID 13237163(2-Ethyl-1,7,10-trioxaspiro[4.6]undecan-2-yl)methanol수율 63.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 3.22 g of 3-chloroperbenzoic acid dissolved in 20 ml of methylene chloride under nitrogen, was added dropwise 3.05 g of tetrahydro-6-(3-methylenepentyl)-1,4-dioxepin-6-ol while maintaining the temperature below 30° C. using a water bath. After six hours and 20 minutes, the reaction mixture was washed with a 25% solution of potassium carbonate and a saturated sodium chloride solution, dried and stripped to yield 2.10 g of the desired product as a dark brown liquid.

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후처리

  1. temperaturewhile maintaining the temperature below 30° C.
  2. wash20 minutes, the reaction mixture was washed with a 25% solution of potassium carbonate
  3. dry with materiala saturated sodium chloride solution, dried

출처 및 근거

ORD 기록
ord-103510cf4a2c4c55975a3bbf649e9e9a
출처 데이터셋
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04410354

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