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

HRID 227895

反応式

HRID 227895 の反応式
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

参加物

4

反応物 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

生成物 1

HCID 57757255HCID 57757255、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

(+)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.

後処理

  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

出典と根拠

ORDレコード
ord-069bb6ea66c24220a267c07d54ed877e
出典データセット
uspto-grants-2009_07
特許番号
US07560597B2

関連ノート

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