Water → HCID 20384467, 화합물

HRID 838790노트

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HRID 838790 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][C:16](=[CH2:18])[CH3:17])=[O:13].O>O1CCCC1.C(OCC)C>[C:12](=[O:13])([O:14][CH2:15][C:16](=[CH2:17])[CH3:18])[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 170604Carbonochloridic acid, 2-methyl-2-propen-1-yl esterHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 20384467HCID 20384467, 화합물수율 94.6%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a solution of 13.94 grams (0.12 mole) of 2,3-dimethylpentan-3-ol in 75 milliliters of anhydrous tetrahydrofuran at 0° C under a nitrogen atmosphere was added with stirring one equivalent of methyllithium in diethyl ether. Then 19.31 grams (0.14 mole) of methallyl chloroformate in 25 milliliters of anhydrous tetrahydrofuran was added. During additions the temperature was maintained at 0° C. Cooling was discontinued and the reaction mixture was stirred for about 18 hours. The reaction mixture was poured into water, and then extracted with ether. The ether layer was separated and washed with water, and then dried over magnesium sulfate. Removal of solvent under reduced pressure yielded 24.32 grams (94.6%) of a yellow oil. A pure sample was obtained by vacuum distillation (Fraction 2).

후처리

  1. temperatureCooling
  2. extractionextracted with ether
  3. customThe ether layer was separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customRemoval of solvent under reduced pressure

출처 및 근거

ORD 기록
ord-627e7d89d7424008841fee1e77b588c0
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04092988

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