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m-Chloroperbenzoic acid → 3-(3,4-Dichlorophenyl)-1,4-oxathiane 4-oxide

HRID 274343
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HRID 274343 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[S:14][CH2:13][CH2:12][O:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].ClC1C=C(C=CC=1)C(OO)=[O:20].C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[S:14](=[O:20])[CH2:13][CH2:12][O:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
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참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 200931953-(3,4-Dichlorophenyl)-1,4-oxathiane

생성물 1

HCID 200931943-(3,4-Dichlorophenyl)-1,4-oxathiane 4-oxide수율 81.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

A stirred solution of 3-(3,4-dichlorophenyl)-1,4-oxathiane (1 g, 4 mmol) in dichloromethane (10 ml) at 0° C. was treated with a solution of meta-chloroperoxybenzoic acid (85%, 860 mg, 4 mmol) in dichloromethane (10 ml) and stirred at 0° C. for 30 mins then at room temperature for 3 hrs. The mixture was shaken with aqueous sodium bicarbonate solution and the organic phase separated, dried (MgSO4) and evaporated to give a solid which was triturated with hexane/toluene (1:1) to give 3-(3,4-dichlorophenyl)-1,4-oxathiane 4-oxide (860 mg), as a colourless crystalline solid, m.p. 100°-103° C.;

후처리

  1. waitat room temperature for 3 hrs
  2. customthe organic phase separated
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customto give a solid which
  6. customwas triturated with hexane/toluene (1:1)

출처 및 근거

ORD 기록
ord-38e2063268b84022afa969a25c867dc9
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05389649

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