Sodium Hydroxide → 3-[2,4,6-Tris-(1-methylethyl)phenyl]-2-propenyl carboxylic acid

HRID 2396290ノート

反応式

HRID 2396290 の反応式
[OH-].[Na+].[CH3:3][CH:4]([C:6]1[CH:11]=[C:10]([CH:12]([CH3:14])[CH3:13])[CH:9]=[C:8]([CH:15]([CH3:17])[CH3:16])[C:7]=1[CH:18]=[CH:19][CH2:20][C:21]([O:23]C)=[O:22])[CH3:5]>CO.O>[CH3:5][CH:4]([C:6]1[CH:11]=[C:10]([CH:12]([CH3:13])[CH3:14])[CH:9]=[C:8]([CH:15]([CH3:16])[CH3:17])[C:7]=1[CH:18]=[CH:19][CH2:20][C:21]([OH:23])=[O:22])[CH3:3]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 867492493-[2,4,6-Tris(1-methylethyl)phenyl]-2-propenyl carboxylic acid, methyl ester

生成物 1

HCID 538822253-[2,4,6-Tris-(1-methylethyl)phenyl]-2-propenyl carboxylic acid収率 88.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Sodium hydroxide (0.23 g, 5.7 mmol) was added to a solution of 3-[2,4,6-tris(1-methylethyl)phenyl]-2-propenyl carboxylic acid, methyl ester (1.5 g, 5.2 mmol) in 100 mL methanol and 10 mL water. Stirred at room temperature for 48 hours and concentrated to dryness. Partitioned theresidue between water and diethyl ether. The aqueous layer was acidified with concentrated HCl and extracted with dichloromethane. The organic extract was dried over MgSO4, filtered, and concentrated to give 1.33g of 3-[2,4,6-tris-(1-methylethyl)phenyl]-2-propenyl carboxylic acid as a white solid, mp 201°-203° C.

後処理

  1. concentrationconcentrated to dryness
  2. customPartitioned
  3. extractionextracted with dichloromethane
  4. extractionThe organic extract
  5. dry with materialwas dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-e50f2cb825134ed3b9c67c90aa71c3d0
出典データセット
uspto-grants-1996_02
特許番号
US05491172

反応ノート

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