Lithium Hydroxide → HCID 13708826、化合物

HRID 326795ノート

反応式

HRID 326795 の反応式
[OH-].[Li+].[CH3:3][C:4](=[CH2:13])/[CH:5]=[CH:6]/[CH2:7][C:8]([O:10]CC)=[O:9]>CO.O1CCCC1.O>[CH3:13][C:4](=[CH2:3])/[CH:5]=[CH:6]/[CH2:7][C:8]([OH:10])=[O:9]

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 14524662Ethyl trans-4-methyl-2,4-pentadienecarboxylate

生成物 1

HCID 13708826HCID 13708826、化合物収率 76%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

2.5 g (0.1 mol) of lithium hydroxide are added at 0° C. to 10 g (0.07 mol) of ethyl trans-4-methyl-2,4-pentadienecarboxylate, dissolved in a solvent mixture of 75 ml of methanol, 17 ml of tetrahydrofuran and 2.5 ml of water, and the mixture is stirred for 20 hours at room temperature. After the mixture has been diluted with 200 ml of water, it is extracted once using diethyl ether, and a pH of 1 is established in the aqueous phase at 0° C. using concentrated hydrochloric acid. The mixture is extracted using diethyl ether, the combined organic phases are washed several times with water and saturated sodium chloride solution, and, after drying and concentrating, 6.1 g (76% of theory) of trans-4-methyl-2,4-pentadienecarboxylic acid are obtained. ##STR207##

後処理

  1. extractionis extracted once using diethyl ether
  2. customis established in the aqueous phase at 0° C.
  3. extractionThe mixture is extracted
  4. washthe combined organic phases are washed several times with water and saturated sodium chloride solution
  5. customafter drying
  6. concentrationconcentrating

出典と根拠

ORDレコード
ord-28cbf9e0b02b4c7db2e5e2a4d4e1c4f2
出典データセット
uspto-grants-1993_12
特許番号
US05270340

反応ノート

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