Ethylene carbonate → HCID 13753176, 화합물

HRID 1732156노트

반응식

HRID 1732156 반응식
[C:1]1(=O)[O:5][CH2:4][CH2:3][O:2]1.[F:7][C:8]1[CH:21]=[CH:20][C:11]([O:12][C:13]2[CH:18]=[CH:17]C(O)=[CH:15][CH:14]=2)=[CH:10][CH:9]=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.CN(C)C=O>[F:7][C:8]1[CH:21]=[CH:20][C:11]([O:12][C:13]2[CH:18]=[CH:17][C:1]([O:5][CH2:4][CH2:3][OH:2])=[CH:15][CH:14]=2)=[CH:10][CH:9]=1

참가 물질

5

반응물 2

HCID 7303Ethylene carbonate2회HCID 129406244-(4-Fluorophenoxy)phenol

생성물 1

HCID 13753176HCID 13753176, 화합물

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 6228Dimethylformamide용매

실험 절차

6.8 g of ethylene carbonate and 2.3 g of tetrabutylammonium bromide are added to a solution of 13.8 g of p-(p-fluorophenoxy)phenol in 35 ml of dimethylformamide. After 4 hours at reflux there are added an additional 1.2 g of ethylene carbonate, and the mixture is heated at reflux for an additional 2 hours. The cooled mixture is poured into 150 ml of ice/water and extracted three times with 100 ml of ethyl acetate each time. The extracts are washed twice with 100 ml of saturated sodium chloride solution each time, dried and evaporated. The residue is purified by recrystallization from n-hexane/ethyl acetate to yield pure 2-[p-(p-fluorophenoxy)-phenoxy]-ethanol, m.p. 74°-76° C.

후처리

  1. temperatureAfter 4 hours at reflux there
  2. temperaturethe mixture is heated
  3. temperatureat reflux for an additional 2 hours
  4. extractionextracted three times with 100 ml of ethyl acetate each time
  5. washThe extracts are washed twice with 100 ml of saturated sodium chloride solution each time
  6. customdried
  7. customevaporated
  8. customThe residue is purified by recrystallization from n-hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-3e2b13758cf642e1984788f8d8ff370c
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04625048

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