1-Bromopentane → 2,5-Bis(pentyloxy)terephthalic acid

HRID 375908

反応式

HRID 375908 の反応式
C([O:3][C:4](=[O:18])[C:5]1[CH:15]=[C:14]([OH:16])[C:8]([C:9]([O:11]CC)=[O:10])=[CH:7][C:6]=1[OH:17])C.C(=O)([O-])[O-].[K+].[K+].Br[CH2:26][CH2:27][CH2:28][CH2:29][CH3:30]>C1(=O)CCCC1.[I-].[K+]>[CH2:26]([O:16][C:14]1[CH:15]=[C:5]([C:4]([OH:3])=[O:18])[C:6]([O:17][CH2:7][CH2:6][CH2:5][CH2:15][CH3:14])=[CH:7][C:8]=1[C:9]([OH:11])=[O:10])[CH2:27][CH2:28][CH2:29][CH3:30]

参加物

6

反応物 3

HCID 80571-BromopentaneHCID 11430Potassium CarbonateHCID 79980Diethyl 2,5-dihydroxyterephthalate

生成物 1

HCID 189913702,5-Bis(pentyloxy)terephthalic acid収率 140.2%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 8452Cyclopentanone溶媒

実験手順

A mixture of 25.4 g of 2,5-dihydroxy terephthalic acid diethyl ester, 30.0 g potassium carbonate, 1 g potassium iodide and 31.5 g 1-bromopentane was heated to boiling-point in cyclopentanone for at least 24 hours. The solvent was withdrawn and 250 ml of 5 wt % caustic potash and 20 ml ethanol was added to the residue, which was then heated to boiling-point for at least 24 hours. After cooling to room temperature the product was precipitated by acidifying with hydrochloric acid and was recrystallized from methylene chloride. 23.7 g of 2,5-bis(pentyloxy) terephthalic acid was obtained.

後処理

  1. temperaturewas heated
  2. customThe solvent was withdrawn
  3. addition250 ml of 5 wt % caustic potash and 20 ml ethanol was added to the residue, which
  4. temperaturewas then heated
  5. waitto boiling-point for at least 24 hours
  6. customwas precipitated
  7. customwas recrystallized from methylene chloride

出典と根拠

ORDレコード
ord-b4542d6c6cea403991b46ee36a21d6ce
出典データセット
uspto-grants-1996_01
特許番号
US05488093

関連ノート

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