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Tetrahydrofuran → HCID 178447715, 화합물

HRID 863727
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HRID 863727 반응식
CC(C)([O-])C.[K+].[Br-].[F:8][C:9]1[CH:10]=[C:11]([CH:32]=[CH:33][C:34]=1[F:35])[CH2:12][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCCC1.[CH2:41]([Si:46]1([C:60]2[CH:65]=[CH:64][CH:63]=[CH:62][CH:61]=2)[CH2:51][CH2:50][CH:49]([CH:52]2[CH2:57][CH2:56][CH:55]([CH:58]=O)[CH2:54][CH2:53]2)[CH2:48][CH2:47]1)[CH2:42][CH2:43][CH2:44][CH3:45]>CCCCCC.O>[F:8][C:9]1[CH:10]=[C:11]([CH:12]=[CH:58][C@H:55]2[CH2:54][CH2:53][C@H:52]([CH:49]3[CH2:48][CH2:47][Si:46]([CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])([C:60]4[CH:61]=[CH:62][CH:63]=[CH:64][CH:65]=4)[CH2:51][CH2:50]3)[CH2:57][CH2:56]2)[CH:32]=[CH:33][C:34]=1[F:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8028Tetrahydrofuran3회HCID 107904853,4-Difluorobenzyltriphenylphosphonium bromideHCID 23665647Potassium tert-butoxideHCID 538633044-(4-Phenyl-4-n-pentyl-4-silacyclohexyl)cyclohexane carbaldehyde

생성물 1

HCID 178447715HCID 178447715, 화합물수율 91%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8058Hexane용매

실험 절차

12.0 g of potassium t-butoxide was added to a mixture of 47.0 g of 3,4-difluorobenzyltriphenylphosphonium bromide and 200 ml of tetrahydrofuran (hereinafter referred to as THF) to obtain an orange-colored ylide solution. 50 ml of a THF solution of 35.0 g of 4-(4-n-pentyl-4-phenyl-4-silacyclohexyl)cyclohexane carbaldehyde was added to the solution, followed by agitation at room temperature for 2 hours. Thereafter, the reaction solution was poured into iced water and extracted with ethyl acetate. The resultant extract was washed with brine, dried and concentrated to obtain a residue, to which 100 ml of n-hexane was added. The resultant crystals of triphenylphosphine oxide were separated by filtration and the resultant filtrate was concentrated. The resultant residue was purified through silica gel chromatography to obtain 41.7 g of 4-(trans-4-(2-(3,4-difluorophenyl)ethenyl)cyclohexyl)-1-n-pentyl-1-phenyl-1-silacyclohexane. This product was subjected to IR analysis with the results shown below.

후처리

  1. customto obtain an orange-colored ylide solution
  2. extractionextracted with ethyl acetate
  3. extractionThe resultant extract
  4. washwas washed with brine
  5. customdried
  6. concentrationconcentrated
  7. customto obtain a residue
  8. customThe resultant crystals of triphenylphosphine oxide were separated by filtration
  9. concentrationthe resultant filtrate was concentrated
  10. customThe resultant residue was purified through silica gel chromatography

출처 및 근거

ORD 기록
ord-07a941a7930e4f90b59e1ec72519987e
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05560866

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