Phosgene → bisphenol TMC 4,4'-dihydroxydiphenyl ether

HRID 30948

反応式

HRID 30948 の反応式
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[C:3]([O:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH:2]=1.[CH3:16][CH:17]1[CH2:22][C:21]([C:30]2[CH:35]=[CH:34][C:33]([OH:36])=[CH:32][CH:31]=2)([C:23]2[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=2)[CH2:20][C:19]([CH3:38])([CH3:37])[CH2:18]1.[OH-].[Na+].C(C1C=CC(O)=CC=1)(C)(C)C.C(Cl)(Cl)=O.C(N1CCCCC1)C>O.C(Cl)Cl>[CH3:16][CH:17]1[CH2:22][C:21]([C:23]2[CH:24]=[CH:25][C:26]([OH:29])=[CH:27][CH:28]=2)([C:30]2[CH:35]=[CH:34][C:33]([OH:36])=[CH:32][CH:31]=2)[CH2:20][C:19]([CH3:37])([CH3:38])[CH2:18]1.[CH:13]1[C:12]([OH:15])=[CH:11][CH:10]=[C:9]([O:8][C:3]2[CH:4]=[CH:5][C:6]([OH:7])=[CH:1][CH:2]=2)[CH:14]=1

参加物

9

反応物 6

HCID 6371PhosgeneHCID 73934-tert-ButylphenolHCID 13007N-EthylpiperidineHCID 14798Sodium Hydroxide2 回HCID 160694,4'-Dihydroxydiphenyl etherHCID 41340354,4'-(3,3,5-Trimethylcyclohexylidene)bis(phenol)

生成物 1

HCID 131727055bisphenol TMC 4,4'-dihydroxydiphenyl ether

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

130 ml of methylene chloride are added to a solution, rendered inert with nitrogen, of 7.077 g (0.035 mol.) of 4,4′-dihydroxydiphenyl ether and 10.87 g (0.035 mol.) of bisphenol TMC as well as 6.16 g (0.154 mol.) of sodium hydroxide in 130 ml of water. In a one-step procedure, 0.368 g (0.0024 mol. or 3.5 mol. % relative to bisphenol) of p-tert.-butylphenol (BUP) are added as chain terminator. At a pH value of 14 and at room temperature, 9.7 ml (13.8 g, 0.14 mol.) of phosgene are added in the course of 10 minutes. In order to prevent the pH value from falling below 12, 25% sodium hydroxide solution was added during the phosgenation. When the phosgenation is complete, and after rinsing with nitrogen, 0.10 ml (0.0007 mol., 1 mol. % relative to bisphenol) of n-ethylpiperidine is added as catalyst, and stirring is then carried out for one hour. The aqueous phase is separated off, and the organic phase is acidified with phosphoric acid and washed with distilled water until neutral and free of salt. Precipitation of the polymer in methanol and drying yield 14.08 g of polycarbonate.

後処理

  1. additionwas added during the phosgenation
  2. additionis added as catalyst
  3. customThe aqueous phase is separated off
  4. washwashed with distilled water until neutral and free of salt
  5. customPrecipitation of the polymer in methanol
  6. dry with materialdrying yield 14.08 g of polycarbonate

出典と根拠

ORDレコード
ord-7311ef6d8dd041a89e2326b3f0fb7878
出典データセット
uspto-grants-2008_09
特許番号
US07425358B2

関連ノート

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