Ethylene carbonate → HCID 13753176、化合物

HRID 1732156ノート

反応式

HRID 1732156 の反応式
[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

参加物

5

反応物 2

HCID 7303Ethylene carbonate2 回HCID 129406244-(4-Fluorophenoxy)phenol

生成物 1

HCID 13753176HCID 13753176、化合物

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e2b13758cf642e1984788f8d8ff370c
出典データセット
uspto-grants-1986_11
特許番号
US04625048

反応ノート

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