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

HRID 1600486

반응식

HRID 1600486 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ba116b91729043b9a898dcb51a79fdc0
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05976558

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