Dimethylformamide → HCID 59593959, 화합물

HRID 2262358노트

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HRID 2262358 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13](O)=[C:12]([F:17])[C:11]=2[F:18])=[C:6]([F:19])[C:5]=1[F:20])[CH3:2].[CH:21]([CH:23]1[CH2:28][CH2:27][CH:26]([CH:29]2[CH2:34][CH2:33][CH:32](CC3C=C(S(O)(=O)=O)C=CC=3C)[CH2:31][CH2:30]2)[CH2:25][CH2:24]1)=[CH2:22].[OH-].[K+].CN(C)[CH:51]=[O:52]>C1(C)C=CC=CC=1.O>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([O:52][CH2:51][CH:32]3[CH2:33][CH2:34][CH:29]([CH:26]4[CH2:25][CH2:24][CH:23]([CH:21]=[CH2:22])[CH2:28][CH2:27]4)[CH2:30][CH2:31]3)=[C:12]([F:17])[C:11]=2[F:18])=[C:6]([F:19])[C:5]=1[F:20])[CH3:2]

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 14797Potassium HydroxideHCID 579529364'-Ethoxy-2,3,2',3'-tetrafluorobiphenyl-4-olHCID 131728572HCID 131728572, 화합물

생성물 1

HCID 59593959HCID 59593959, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

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온도
60 °C

실험 절차

In a reactor under nitrogen atmosphere, 4.0 g of compound (a4), 5.3 g of compound (a6) and 1.2 g of potassium hydroxide (KOH) were added into 30 ml of N,N-dimethylformamide (DMF), followed by stirring at 60° C. for 14 hours. The reaction solution was cooled to 30° C., to which 100 ml of water and 100 ml of toluene were added. The mixture was separated into organic layer and aqueous layer and the organic layer was extracted. The resulting organic layer was separated and washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to provide the residue. The resulting residue was purified by column chromatography (silica gel; toluene), further purified by recrystallization from (volume ratio Solmix A-11: toluene=1:2), dried to provide 2.5 g of 4′-ethoxy-2,3,2′,3′-tetrafluoro-4-(4′-vinylbicyclohexyl-4-ylmetoxy)-biphenyl (a7).

후처리

  1. additionwere added
  2. customThe mixture was separated into organic layer and aqueous layer
  3. extractionthe organic layer was extracted
  4. customThe resulting organic layer was separated
  5. washwashed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customto provide the residue
  9. customThe resulting residue was purified by column chromatography (silica gel; toluene)
  10. customfurther purified by recrystallization from (volume ratio Solmix A-11: toluene=1:2)
  11. customdried

출처 및 근거

ORD 기록
ord-204c22dccac64c5ba79c1cda2c330272
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851032B2

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