Toluene → 2-Tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane

HRID 247357

반응식

HRID 247357 반응식
[CH3:1][C:2]([OH:10])([CH2:4][CH2:5][C:6]([CH3:9])([OH:8])[CH3:7])[CH3:3].[CH:11](=O)[C:12]([CH3:15])([CH3:14])[CH3:13].C1(C)C=CC=CC=1>C1(C)C=CC(S(O)(=O)=O)=CC=1.O>[C:12]([CH:15]1[O:10][C:2]([CH3:3])([CH3:1])[CH2:4][CH2:5][C:6]([CH3:9])([CH3:7])[O:8]1)([CH3:14])([CH3:13])[CH3:11]

참가 물질

6

반응물 3

HCID 1140TolueneHCID 80312,5-Dimethyl-2,5-hexanediolHCID 12417Pivalaldehyde

생성물 1

HCID 139807482-Tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane수율 85%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 962Water용매

실험 절차

A mixture of 730 g (5 mol) of 2,5-dimethylhexane-2,5-diol, 3 g of p-toluenesulfonic acid, 430 g (5 mol) of pivalaldehyde and 1 l of toluene was refluxed for 4 hours (h) during which the water of reaction produced (90 ml) was removed. The reaction mixture was then cooled down to room temperature (RT) and stirred up with 10 ml of 25% strength aqueous sodium hydroxide solution, the phases were separated, the organic phase was washed with a little water until neutral, and the toluene was then removed at 50°-60° C. The residue obtained was fractionated under reduced pressure affording 909 g (4.25 mol) of 2-tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane (boiling point 54° C./0.2 mbar). This corresponds to a yield of 85% of theory.

후처리

  1. temperaturewas refluxed for 4 hours (h) during which
  2. customproduced (90 ml)
  3. customwas removed
  4. customthe phases were separated
  5. washthe organic phase was washed with a little water until neutral, and the toluene
  6. customwas then removed at 50°-60° C
  7. customThe residue obtained

출처 및 근거

ORD 기록
ord-03ed008d92b34129a4600f2fd633702e
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04707302

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