Phenol → Bisphenol A

HRID 2112367

반응식

HRID 2112367 반응식
[C:1]1([CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[CH:3]=1)O.C[N+](CCCC)(CCCC)[CH2:11][CH2:12][CH2:13]C.[OH-].[Na+].[C:25]1([OH:31])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(Cl)(Cl)=O>O.C(N(CC)CC)C.C(Cl)Cl>[CH3:11][C:12]([C:28]1[CH:27]=[CH:26][C:25]([OH:31])=[CH:30][CH:29]=1)([C:8]1[CH:1]=[CH:3][C:4]([OH:5])=[CH:6][CH:7]=1)[CH3:13]

참가 물질

9

반응물 5

HCID 996PhenolHCID 5054ResorcinolHCID 6371PhosgeneHCID 14798Sodium HydroxideHCID 36209Tributylmethylammonium

생성물 1

HCID 6623Bisphenol A

시약·촉매·용매 3

HCID 962Water용매2회HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

Into a 500 ml Morton flask equipped with a mechanical stirrer, a reflux condenser, a nitrogen bypass, a pH probe and a phosgene dip tube was placed 6.88 g of resorcinol, 100 ml of methylene chloride, 20 ml of water and 0.5 ml of 75 wt % aqueous methyltributylammonium (MTBA). The pH was adjusted to and maintained at 7 with 25 wt % of NaOH as 29 g of a 35 wt % solution of diacid chlorides (DACS) in methylene chloride (delivers 50 mmol of 50/50 isophthaloyl chloride (IPC)/terephthaloyl chloride (TPC)) was added over 4 minutes. The pH was raised to 10 and 100 μl of triethylamine (TEA), 50 mg of water and 0.21 g of phenol were added. The pH was maintained at 10 and 4.0 g of phosgene was added at 0.5 g/min. The final pH was 10.1. The polymer solution was separated from the brine by centrifugation and washed 1 time with 1N HCl and 3 times with deionized water. The polymer was isolated by hot water crumbing in a blender and collected by filtration and washed with water and dried in a vacuum oven at 110° C. overnight.

후처리

  1. customInto a 500 ml Morton flask equipped with a mechanical stirrer, a reflux condenser
  2. additionwas added over 4 minutes
  3. additionwere added
  4. additionwas added at 0.5 g/min
  5. customThe polymer solution was separated from the brine by centrifugation
  6. washwashed 1 time with 1N HCl and 3 times with deionized water
  7. customThe polymer was isolated by hot water crumbing in a blender
  8. filtrationcollected by filtration
  9. washwashed with water
  10. customdried in a vacuum oven at 110° C. overnight

출처 및 근거

ORD 기록
ord-fc1d59adaf3240b586343ea1f382c981
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07524562B2

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