Acetic Acid → 2-(7-Oxooctyl)isoindoline-1,3-dione

HRID 1164494노트

반응식

HRID 1164494 반응식
[O:1]=[C:2]([CH3:25])[CH:3](C(OCC)=O)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:11]2[C:10]1=[O:19].C(O)(=O)C.Cl.O>C(Cl)Cl.[OH-].[Na+]>[O:1]=[C:2]([CH3:25])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][N:9]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:11]2[C:10]1=[O:19]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 962WaterHCID 13801454N-[7-Oxo(6-carboethoxy)octyl]phthalimide

생성물 1

HCID 205113062-(7-Oxooctyl)isoindoline-1,3-dione

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 350 g of crude N-[7-oxo(6-carboethoxy)octyl]phthalimide and 1000 ml of acetic acid, concentrated hydrochloric acid, and water was refluxed for three hours. The reaction mixture was stripped, the residue dissolved in methylene chloride and basified with 2 N NaOH solution. The organic layer was separated, dried over anhydrous sodium sulfate, filtered and stripped to an orange oil, 73% pure by gc (SE-30, 90-280°@16°/min). This material was used without further purification in Preparation 3.

후처리

  1. temperaturewas refluxed for three hours
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customstripped to an orange oil, 73% pure by gc (SE-30, 90-280°@16°/min)
  6. customThis material was used without further purification in Preparation 3

출처 및 근거

ORD 기록
ord-6f5c6ae26ff246d7a6a14057ba10a250
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04370335

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