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Thiophenol → HCID 13252413, 화합물

HRID 647407
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HRID 647407 반응식
Cl[CH:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[C:4](=[O:11])[N:3]1[C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1[F:19].[C:20]1([SH:26])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)CC)C>ClCCl>[Cl:18][C:15]1[CH:16]=[CH:17][C:12]([N:3]2[CH:2]([S:26][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:10]3[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=3[C:4]2=[O:11])=[C:13]([F:19])[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7969ThiophenolHCID 8471TriethylamineHCID 132576323-Chloro-2-(4-chloro-2-fluorophenyl)-2,3,4,5,6,7-hexahydro-1H-isoindol-1-one

생성물 1

HCID 13252413HCID 13252413, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 30 ml of dichloromethane were dissolved 3.0 g of 3-chloro-2-(4-chloro-2-fluorophenyl)-2,3,4,5,6,7-hexahydro-1H-isoindol-1-one and 1.1 g of thiophenol, and 1.0 g of triethylamine was added to the solution over a 10-minute period, followed by stirring at room temperature for 2 hours. The reaction mixture was washed with water, dried over anhydrous sodium sulfate and freed of the dichloromethane under reduced pressure. The residue was purified by means of column chromatography with the use of silica gel (developing solvent of dichloromethaneacetone), thereby producing 3.2 g (yield of 86%) of the subject compound in white crystals, m.p. 86°-87° C.

후처리

  1. additionwas added to the solution over a 10-minute period
  2. washThe reaction mixture was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe residue was purified by means of column chromatography with the use of silica gel (developing solvent of dichloromethaneacetone)

출처 및 근거

ORD 기록
ord-a77da4258fe1423584ede4039290dd44
출처 데이터셋
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04409018

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