Dichloromethane → HCID 178515546、化合物

HRID 224681ノート

反応式

HRID 224681 の反応式
O[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:11]2C=CC(O)=CC=2)(C)C)=[CH:4][CH:3]=1.C(Cl)Cl.[C:21](Cl)(Cl)=[O:22].C([N:27](CC)CC)C>[OH-].[Na+]>[OH:22][C:21]1[CH:11]=[CH:8][C:5]2[C:4](=[CH:3][CH:2]=[CH:7][CH:6]=2)[N:27]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 6371PhosgeneHCID 6623Bisphenol AHCID 8471Triethylamine

生成物 1

HCID 178515546HCID 178515546、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒2 回

実験手順

456 g of bisphenol A and 559 g of 2-[4-hydroxyphenyl]-2-[5-(8-hydroxyquinolyl)]-propane are dissolved in 4 kg of 9% strength sodium hydroxide solution and 9 kg of methylene chloride are then added. 562.8 g of phosgene are introduced with vigorous stirring and 60 ml of a 4% strength triethylamine solution are then added dropwise. The mixture is stirred for a further hour and if necessary sufficient sodium hydroxide solution is added for the pH of the solution to remain constant at 13. The phases are separated and the aqueous phase is tested for complete conversion. The organic phase is extracted once with 5% strength H3PO4, washed with water until neutral and subsequently dried over sodium-sulphate. The organic phase is concentrated and the short-chain polycarbonate with hydroxyquinoline end groups is obtained direct by precipitation in methanol. ηrel : 1.038 (ηrel is measured in CH2Cl2 at 20° C.; 0.5 g solved in 100 g solution); nitrogen analysis: N2 2.56%; phenolic OH: 2.8%. The molecular weight calculated from these values is Mn =1178.

後処理

  1. additionare then added
  2. additionis added for the pH of the solution
  3. customThe phases are separated
  4. extractionThe organic phase is extracted once with 5% strength H3PO4
  5. washwashed with water until neutral and
  6. dry with materialsubsequently dried over sodium-sulphate
  7. concentrationThe organic phase is concentrated

出典と根拠

ORDレコード
ord-2ecfdb2cb15c4e808c6a36ce6af57afb
出典データセット
uspto-grants-1980_11
特許番号
US04233431

反応ノート

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