Water → HCID 20384467、化合物

HRID 838790ノート

反応式

HRID 838790 の反応式
[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]

参加物

7

反応物 4

HCID 962WaterHCID 116852,3-Dimethylpentan-3-olHCID 170604Carbonochloridic acid, 2-methyl-2-propen-1-yl esterHCID 178418348HCID 178418348、化合物

生成物 1

HCID 20384467HCID 20384467、化合物収率 94.6%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-627e7d89d7424008841fee1e77b588c0
出典データセット
uspto-grants-1978_06
特許番号
US04092988

反応ノート

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