Sodium Iodide → 4-(3-Iodopropoxy)benzoic acid, methyl ester

HRID 1780786노트

반응식

HRID 1780786 반응식
S1C2C=CC=CC=2N=C1C(C1CCN([CH2:18][CH2:19][CH2:20][O:21][C:22]2[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=2)CC1)=O.ClCCCOC1C=CC(C(OC)=O)=CC=1.[I-:47].[Na+]>CC(C)=O.C(OCC)C>[I:47][CH2:18][CH2:19][CH2:20][O:21][C:22]1[CH:31]=[CH:30][C:25]([C:26]([O:28][CH3:29])=[O:27])=[CH:24][CH:23]=1

참가 물질

6

반응물 3

HCID 5238Sodium IodideHCID 12389265Methyl 4-(3-chloropropoxy)benzoateHCID 153374634-[3-[4-[(2-Benzothiazolyl)carbonyl]-1-piperidinyl]propoxy]benzoic acid methyl ester

생성물 1

HCID 153374624-(3-Iodopropoxy)benzoic acid, methyl ester

시약·촉매·용매 2

HCID 180Acetone용매HCID 3283Diethyl Ether용매

실험 절차

4-[3-[4-[(2-Benzothiazolyl)carbonyl]-1-piperidinyl]propoxy]benzoic acid, methyl ester ##STR22## Dissolve 4-(3-chloropropoxy)benzoic acid, methyl ester (6.97 g, 30.5 mmol) in anhydrous acetone (100 mL) and add powdered sodium iodide (16.0 g, 107 mmol). Heat at reflux under an argon atmosphere for 38 hours. Dilute with ethyl ether (100 mL) and filter through Celite® filter aid. Wash the filtrate with water and brine, then dry (MgSO4). Evaporate the solvent in vacuo to give 4-(3-iodopropoxy)benzoic acid, methyl ester as a yellow oil.

후처리

  1. temperatureHeat
  2. temperatureat reflux under an argon atmosphere for 38 hours
  3. filtrationfilter through Celite®
  4. filtrationfilter aid
  5. washWash the filtrate with water and brine
  6. dry with materialdry (MgSO4)
  7. customEvaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-b55a5b56ecd6472eb1f52e0aa86fe4a7
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05631268

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