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p-Chlorothiophenol → 6-(4-Chlorophenylsulfanyl)-hexylphthalimide

HRID 2097361
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HRID 2097361 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.BrCCCCCC[N:16]1[C:20](=[O:21])[C:19]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:18]2[C:17]1=[O:26].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:6][CH2:7][CH2:2][CH2:3][CH2:4][CH2:5][C:25]2[CH:24]=[CH:23][CH:22]=[C:19]3[C:20]([NH:16][C:17](=[O:26])[C:18]=23)=[O:21])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 141120N-(6-Bromohexyl)phthalimide

생성물 1

HCID 866225746-(4-Chlorophenylsulfanyl)-hexylphthalimide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

4-Chlorothiophenol (2.89 g, 20 mmol), N-(6-bromohexyl)-phthalimide (6.20 g, 20 mmol) and K2CO3 (5.53 g, 40 mmol) were suspended in DMF (50 mL) under an atmosphere of argon and stirred at 90° C. for 23 h. The solvent was evaporated under reduced pressure and the residue was partitioned between water (100 mL) and CH2Cl2 (150 mL). The aqueous layer was extracted with CH2Cl2 (2×100 mL), the combined org. layers were dried over Na2SO4, filtered and the solvent was removed under reduced pressure to give the title compound, pure enough for further reactions.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was partitioned between water (100 mL) and CH2Cl2 (150 mL)
  3. extractionThe aqueous layer was extracted with CH2Cl2 (2×100 mL)
  4. dry with materiallayers were dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-2987f79b79ab4f438c4117417e1cc34e
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450348B2

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