4-Hydroxybiphenyl → 4-(8-Hydroxyoctyl)oxybiphenyl

HRID 256498

반응식

HRID 256498 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][OH:10].[C:11]1([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[OH-].[Na+]>[Cl-].C[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC.O.O1CCCC1>[C:17]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:18]=[CH:19][C:20]([O:23][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][OH:10])=[CH:21][CH:22]=1

참가 물질

7

반응물 3

HCID 71034-HydroxybiphenylHCID 14798Sodium HydroxideHCID 1626071-Octanol, 8-bromo-

생성물 1

HCID 139591154-(8-Hydroxyoctyl)oxybiphenyl수율 65.4%

시약·촉매·용매 3

HCID 21218Trioctylmethylammonium chloride촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 37.8 g of 8-bromo-1-octanol, 30.77 g of 4-phenylphenol, 8.31 g of sodium hydroxide and 34 g of N--methyl-N,N--dioctyl-1-octanaminium chloride in 100 ml of water and 175 ml of tetrahydrofuran was refluxed for 17 hours. The tetrahydrofuran was removed and the residue extracted with warm chloroform. The chloroform extract was washed with water, dried and the solvent removed. The residue was recrystallized from methanol, giving 35.26 g of the desired compound as a white solid, mp 101°-103° C.

후처리

  1. temperaturewas refluxed for 17 hours
  2. customThe tetrahydrofuran was removed
  3. extractionthe residue extracted with warm chloroform
  4. extractionThe chloroform extract
  5. washwas washed with water
  6. customdried
  7. customthe solvent removed
  8. customThe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-ef4b0c88312a4ec6908e3248d17efc7c
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04703130

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