Chlorobis(2,6,6-trimethylbicyclo[3.1.1]heptan-3-yl)borane → HCID 57757255, 화합물

HRID 227895

반응식

HRID 227895 반응식
B(Cl)([C@@H]1[C@@H](C)[C@@H]2C(C)(C)[C@@H](C2)C1)[C@@H]1[C@@H](C)[C@@H]2C(C)(C)[C@@H](C2)C1.[Cl:23][C:24]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:25]=1[C:31]1[CH:36]=[CH:35][C:34]([C:37](=[O:43])[CH2:38][CH2:39][CH2:40][CH:41]=[CH2:42])=[CH:33][CH:32]=1>CCOCC>[Cl:23][C:24]1[CH:29]=[C:28]([Cl:30])[CH:27]=[CH:26][C:25]=1[C:31]1[CH:36]=[CH:35][C:34]([C@H:37]([OH:43])[CH2:38][CH2:39][CH2:40][CH:41]=[CH2:42])=[CH:33][CH:32]=1

참가 물질

4

반응물 2

HCID 13515837Chlorobis(2,6,6-trimethylbicyclo[3.1.1]heptan-3-yl)boraneHCID 577572631-(2',4'-Dichloro-biphenyl-4-yl)-hex-5-en-1-one

생성물 1

HCID 57757255HCID 57757255, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

(+)DIP-Chloride (2.4 g) was dissolved in dry ether (10 mL) and cooled in an ethanol/CO2 bath. 1-(2′,4′-Dichloro-biphenyl-4-yl)-hex-5-en-1-one (1 g) was dissolved in dry ether (5 mL) and added dropwise to the DIP solution. The mixture was allowed to warm to room temperature and stirred for 24 hours. Petrol (50 mL) was added and the organic layer was separated. The aqueous layer was diluted with water and extracted with a further 50 mL petrol. The organics were combined, dried and evaporated to give a thick oil. It was not possible to obtain a pure sample by column chromatography, but no trace of starting material remained, as assessed by thin layer chromatography.

후처리

  1. temperaturecooled in an ethanol/CO2 bath
  2. additionadded dropwise to the DIP solution
  3. customthe organic layer was separated
  4. additionThe aqueous layer was diluted with water
  5. extractionextracted with a further 50 mL petrol
  6. customdried
  7. customevaporated
  8. customto give a thick oil
  9. customto obtain a pure sample by column chromatography

출처 및 근거

ORD 기록
ord-069bb6ea66c24220a267c07d54ed877e
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560597B2

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