2,2-Dimethoxypropane → HCID 86588954、化合物

HRID 900495ノート

反応式

HRID 900495 の反応式
O[CH2:2][CH2:3][C@H:4](O)[C:5]([CH3:9])([CH3:8])[C:6]#[N:7].C12(CS(O)(=O)=O)C(C)(C)C(CC1)CC2=O.[CH3:26][O:27][C:28]([O:31][CH3:32])([CH3:30])[CH3:29]>>[CH3:26][O:27][C:28]([O:31][CH3:32])([CH3:30])[CH3:29].[CH3:8][C:5]([CH3:9])([CH2:4][CH2:3][CH3:2])[C:6]#[N:7]

参加物

4

反応物 3

HCID 64952,2-DimethoxypropaneHCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 9833987HCID 9833987、化合物2 回

生成物 1

HCID 86588954HCID 86588954、化合物

実験手順

6.73 g (47 mmol) of 5-hydroxy-2,2-dimethyl-3(S)-hydroxy-pentane-nitrile of the title compound of Example 1d is dissolved in 27 ml of acetone dimethylketal, and 546 mg of camphor-10-sulfonic acid is added. It is heated for 15 hours to 50° C. It is evaporated to the dry state in a vacuum. The residue is taken up in 200 ml of methylene chloride and washed with saturated sodium bicarbonate solution and then with saturated sodium chloride solution. The organic phase is dried on sodium sulfate and evaporated to the dry state in a vacuum. The oil that is obtained crystallizes while standing.

後処理

  1. temperatureIt is heated for 15 hours to 50° C
  2. customIt is evaporated to the dry state in a vacuum
  3. washwashed with saturated sodium bicarbonate solution
  4. customThe organic phase is dried on sodium sulfate
  5. customevaporated to the dry state in a vacuum
  6. customThe oil that is obtained
  7. customcrystallizes

出典と根拠

ORDレコード
ord-c4202dc56e9c4fbe94dfb4220b7179da
出典データセット
uspto-grants-2008_04
特許番号
US07358382B2

反応ノート

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