Ethyl Bromide → Diethyl 2-hydroxybenzene-1,4-dicarboxylate

HRID 128841

반응식

HRID 128841 반응식
N12CCCNC1CCC[CH:3]=[CH:2]2.[OH:12][C:13]1[CH:21]=[C:20]([C:22]([OH:24])=[O:23])[CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16].Br[C:26]1C=C(C(O)=O)C=C[C:27]=1C(O)=O.BrCC>C1C=CC=CC=1>[OH:12][C:13]1[CH:21]=[C:20]([C:22]([O:24][CH2:26][CH3:27])=[O:23])[CH:19]=[CH:18][C:14]=1[C:15]([O:17][CH2:2][CH3:3])=[O:16]

참가 물질

6

반응물 4

HCID 6332Ethyl BromideHCID 68513Bromoterephthalic acidHCID 972572-Hydroxyterephthalic acidHCID 98128211,8-Diazabicyclo[5.4.0]undec-2-ene

생성물 1

HCID 22401614Diethyl 2-hydroxybenzene-1,4-dicarboxylate

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

6.62 g 1,8-diazabicyclo[5.4.0]undecene and 100 mL benzene were added to 3.76 g hydroxyterephthalic acid (synthesized from bromoterephthalic acid by a known method) and the mixture was heated. 6.76 g bromoethane dissolved in 38 mL benzene was added dropwise in and the reaction mixture was heated under reflux for 19 hours. The salt product was filtered off, and purification by column chromatography then yielded 4.66 g diethyl hydroxyterephthalate.

후처리

  1. temperaturewas heated
  2. additionwas added dropwise in and the reaction mixture
  3. temperaturewas heated
  4. temperatureunder reflux for 19 hours
  5. filtrationThe salt product was filtered off
  6. custompurification by column chromatography

출처 및 근거

ORD 기록
ord-7b7a8385411543789c3d9d2e8412d525
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05464922

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