Propanal → HCID 178459257、化合物

HRID 1968946ノート

反応式

HRID 1968946 の反応式
[CH:1](=[O:4])[CH2:2][CH3:3].CC([Si](C)(C)O[C@H:11]1[CH2:16][CH2:15][C@H:14]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:13][CH2:12]1)(C)C.[Bi](Br)(Br)Br.C([SiH](CC)CC)C>C(#N)C>[CH2:1]([O:4][C@H:11]1[CH2:16][CH2:15][C@H:14]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:13][CH2:12]1)[CH2:2][CH3:3]

参加物

6

反応物 4

HCID 527PropanalHCID 12052TriethylsilaneHCID 82232bismuth(III) bromideHCID 178472501HCID 178472501、化合物

生成物 1

HCID 178459257HCID 178459257、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

Propionaldehyde (6.4 g) in acetonitrile (50 mL) was added over 30 minutes to a solution of cis/trans ethyl 4-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}cyclohexanecarboxylate (D1, 25.2 g), bismuth tribromide (4.4 g) and triethylsilane (17.5 mL) in acetonitrile (300 mL) and the mixture was stirred for a further 1.5 hours. The solvent was partially removed then the residue was treated with ethyl acetate and saturated sodium bicarbonate solution. The organic layer was separated, washed with brine, dried with anhydrous sodium sulphate and the solvent was removed to give the title compounds contaminated with silicone residues (39.1 g).

後処理

  1. customThe solvent was partially removed
  2. additionthe residue was treated with ethyl acetate and saturated sodium bicarbonate solution
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried with anhydrous sodium sulphate
  6. customthe solvent was removed

出典と根拠

ORDレコード
ord-233e234679114ce8863c8491940f4efb
出典データセット
uspto-grants-2013_04
特許番号
US08426443B2

反応ノート

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