3,5-Dihydroxybenzoic Acid → HCID 15806381、化合物

HRID 383057

反応式

HRID 383057 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([OH:11])[CH:10]=1)[C:5]([OH:7])=[O:6].C(=O)([O-])[O-].[K+].[K+].[CH2:18](Br)[CH:19]=[CH2:20]>CN(C)C=O>[CH2:18]([O:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:11][CH2:8][CH:4]=[CH2:5])[CH:10]=1)[C:5]([O:7][CH2:3][CH:2]=[CH2:10])=[O:6])[CH:19]=[CH2:20]

参加物

5

反応物 3

HCID 74243,5-Dihydroxybenzoic AcidHCID 7841Allyl bromideHCID 11430Potassium Carbonate

生成物 1

HCID 15806381HCID 15806381、化合物収率 173.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

3,5-Dihydroxybenzoic acid (15.0 g, 97.3 mmol) and potassium carbonate (44.0 g, mol) were mixed in N,N-dimethylformamide (60 ml) and heated to 80° C. Allyl bromide (42.0 g, 0.35 mol) was added dropwise during 1 h and efficient stirring was continued for 24 h. The reaction mixture was then evaporated to a semisolid residue, which was treated with chloroform (500 ml) and filtered. The filtrate was washed with water (3×150 ml), dried (Na2SO4) and filtered through a short column of alumina. Evaporation of the solvent gave 23.1 g (87%) of the product as a colorless oil.

後処理

  1. customThe reaction mixture was then evaporated to a semisolid residue, which
  2. additionwas treated with chloroform (500 ml)
  3. filtrationfiltered
  4. washThe filtrate was washed with water (3×150 ml)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered through a short column of alumina
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-944fee81fa3644c496d92b4937a58c5f
出典データセット
uspto-grants-2001_10
特許番号
US06310243B1

関連ノート

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