Water → 2,3-Dimethylpent-3-yl allyl carbonate

HRID 838789노트

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HRID 838789 반응식
[CH3:1][CH:2]([C:4]([CH3:8])([OH:7])[CH2:5][CH3:6])[CH3:3].C[Li].Cl[C:12]([O:14][CH2:15][CH:16]=[CH2:17])=[O:13].O>O1CCCC1.C(OCC)C>[C:12](=[O:13])([O:14][CH2:15][CH:16]=[CH2:17])[O:7][C:4]([CH3:8])([CH2:5][CH3:6])[CH:2]([CH3:3])[CH3:1]

참가 물질

7

반응물 4

HCID 962WaterHCID 116852,3-Dimethylpentan-3-olHCID 18052Allyl chloroformateHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 203844702,3-Dimethylpent-3-yl allyl carbonate수율 53.9%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a solution of 11.62 grams (0.1 mole) of 2,3-dimethylpentan-3-ol in 75 milliliters of anhydrous tetrahydrofuran at 0° C was added one equivalent of methyllithium in diethyl ether, followed by 12.1 grams (0.10 mole) of allyl chloroformate in 25 milliliters of anhydrous tetrahydrofuran. During both additions the temperature was maintained at 0° C. After the last addition was complete the reaction mixture was stirred for about 18 hours and allowed to warm to ambient temperature. The reaction mixture was poured into water, and then extracted with ether. The ether solution was washed four times with water and dried over magnesium sulfate. Removal of solvent under reduced pressure yielded 18.27 grams (93.1% crude yield) of a yellow oil. Vacuum distillation gave 10.79 grams of 2,3-dimethylpent-3-yl allyl carbonate, b.p. 59°-60° C/0.15 mm.

후처리

  1. additionAfter the last addition
  2. temperatureto warm to ambient temperature
  3. extractionextracted with ether
  4. washThe ether solution was washed four times with water
  5. dry with materialdried over magnesium sulfate
  6. customRemoval of solvent under reduced pressure
  7. customyielded 18.27 grams (93.1% crude yield) of a yellow oil
  8. distillationVacuum distillation

출처 및 근거

ORD 기록
ord-ab4cdb8115e948d8b76618b248b2a44c
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04092988

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