2,2-Dimethoxypropane → HCID 86588954, 화합물

HRID 1797394노트

반응식

HRID 1797394 반응식
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]

참가 물질

4

반응물 3

HCID 64952,2-DimethoxypropaneHCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 9833987HCID 9833987, 화합물2회

생성물 1

HCID 86588954HCID 86588954, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fd551ca1fb07467faecd1a9cff40e391
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07034165B2

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