Potassium Carbonate → Benzyl 2-hydroxy-4-(2-methylallyloxy)benzoate

HRID 1075366

反応式

HRID 1075366 の反応式
[OH:1][C:2]1[CH:17]=[C:16]([OH:18])[CH:15]=[CH:14][C:3]=1[C:4]([O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:5].[C:19](=O)([O-])[O-].[K+].[K+].C[CH:26]=[CH:27][CH2:28]Cl>CN(C=O)C>[OH:1][C:2]1[CH:17]=[C:16]([O:18][CH2:19][C:27]([CH3:28])=[CH2:26])[CH:15]=[CH:14][C:3]=1[C:4]([O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:5]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11589Crotyl chlorideHCID 7500968Benzyl 2,4-dihydroxybenzoate

生成物 1

HCID 21829741Benzyl 2-hydroxy-4-(2-methylallyloxy)benzoate収率 57.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

To a mixture of 17 g of benzyl 2,4-dihydroxybenzoate (0.07 mol) and 10 g of potassium carbonate (0.077 mol) in 60 ml of DMF brought to 70° C. were added 6.81 ml of methyallyl chloride (0.07 mol) dropwise over 1 hour. The mixture was left at 70° C. for 2 hours. It is cooled to about 40° C. and the salts are filtered off. The salts were washed with DMF. The liquids were combined, and the solvent was evaporated off. A brown oil was obtained which was purified on silica (eluent: 70/30 heptane/CH2Cl2). The head fractions were pooled to give 12 g (yield: 57%) of benzyl 2-hydroxy-4-(2-methylallyloxy)benzoate in the form of a colourless oil.

後処理

  1. custombrought to 70° C.
  2. filtrationthe salts are filtered off
  3. washThe salts were washed with DMF
  4. customthe solvent was evaporated off
  5. customA brown oil was obtained which
  6. customwas purified on silica (eluent: 70/30 heptane/CH2Cl2)

出典と根拠

ORDレコード
ord-48e2d24803764d579445d0437df97322
出典データセット
uspto-grants-1999_05
特許番号
US05900231

関連ノート

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