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

HRID 1780786ノート

反応式

HRID 1780786 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b55a5b56ecd6472eb1f52e0aa86fe4a7
出典データセット
uspto-grants-1997_05
特許番号
US05631268

反応ノート

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