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m-Chloroperbenzoic acid → 2-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane-5-oxide

HRID 727865
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HRID 727865 반응식
[F:1][C:2]1[CH:21]=[CH:20][C:5]([C:6](=[C:14]2[S:19][CH2:18][S:17][CH2:16][S:15]2)[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.ClC1C=CC=C(C(OO)=[O:30])C=1>ClCCl>[F:13][C:10]1[CH:9]=[CH:8][C:7]([C:6](=[C:14]2[S:15][CH2:16][S:17](=[O:30])[CH2:18][S:19]2)[C:5]2[CH:20]=[CH:21][C:2]([F:1])=[CH:3][CH:4]=2)=[CH:12][CH:11]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 143292842-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane

생성물 1

HCID 143293802-(4,4'-Difluorobenzhydrylidene)-1,3,5-trithiane-5-oxide수율 76.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a 30 ml of dichloromethane of 1.5 g of 2-(4,4'-difluorobenzhydrylidene)-1,3,5-trithiane was added 0.77 g of m-chloroperbenzoic acid in small portions at 0° C., and the resulting mixture was stirred overnight. After completion of the reaction, the reaction mixture was poured into ice-water and extracted with dichloromethane. Usual work up gave crude solid, which was purified by a silica gel column chromatography (chloroform:hexane=3:1) to obtain 1.2 g of white crystals.

후처리

  1. customAfter completion of the reaction
  2. extractionextracted with dichloromethane
  3. customUsual work up gave crude solid, which
  4. customwas purified by a silica gel column chromatography (chloroform:hexane=3:1)

출처 및 근거

ORD 기록
ord-4357d9e2519b4125be3d40119f892078
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05045562

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