Calcium hypochlorite → 3-Undecanone

HRID 1789572

반응식

HRID 1789572 반응식
C(=O)(O)[O-].[Na+].[CH3:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]([OH:17])[CH2:15][CH3:16].Cl[O-].[Ca+2].Cl[O-]>C(#N)C>[CH3:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14](=[O:17])[CH2:15][CH3:16]

참가 물질

5

반응물 3

HCID 24504Calcium hypochloriteHCID 98970Undecan-3-olHCID 516892Sodium Bicarbonate

생성물 1

HCID 751893-Undecanone

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Sodium bicarbonate (8.81 g, 0.105 mol) was added to a solution of 15.0 g (0.075 mol) of 3,3-dimethyl-1,5-dioxaspiro<5.5>undecan-9-ol in 150 ml of acetonitrile. The reaction mixture was charged with 15.0 g of silica gel (MCB 60-200 mesh) and 15.0 g of calcium hypochlorite in sequence. The reaction mixture was stirred at a temperature in the range of 24° C. to 28° C. for about 18 hours and then warmed to 29° C. to 30° C. for 4 hours. The mixture was filtered and evaporated under vacuum. The residue was combined with 135 ml of toluene and 50 ml of water, and the resulting mixture was stirred for 45 minutes. The organic phase was separated, washed with 50 ml of a saturated sodium chloride solution and dried over 10.0 g of anhydrous sodium sulfate. A gas chromatograph of the sample showed 93.6% pure product. The organic phase was concentrated under vacuum to afford 13.97 g of 3,3-dimethyl-1,5-dioxaspiro<5.5>undecan-9-one.

후처리

  1. temperaturewarmed to 29° C. to 30° C. for 4 hours
  2. filtrationThe mixture was filtered
  3. customevaporated under vacuum
  4. stirringthe resulting mixture was stirred for 45 minutes
  5. customThe organic phase was separated
  6. washwashed with 50 ml of a saturated sodium chloride solution
  7. dry with materialdried over 10.0 g of anhydrous sodium sulfate
  8. concentrationThe organic phase was concentrated under vacuum

출처 및 근거

ORD 기록
ord-8693a1c2b895400fbdf2e6cab0d8b68e
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689415

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