Sodium hydride → 1-[3-(3-benzyloxyphenyl)propyl]-1H-1,2,3-triazole

HRID 2084376ノート

反応式

HRID 2084376 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[N:2]1.[H-].[Na+].I[CH2:9][CH2:10][CH2:11][C:12]1[CH:13]=[C:14]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:16][CH:17]=1>CN(C=O)C.C(OCC)(=O)C>[CH2:19]([O:18][C:14]1[CH:13]=[C:12]([CH2:11][CH2:10][CH2:9][N:1]2[CH:5]=[CH:4][N:3]=[N:2]2)[CH:17]=[CH:16][CH:15]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 22733348Benzyl 3-(3-iodopropyl)phenyl etherHCID 178418936HCID 178418936、化合物

生成物 1

HCID 121098701-[3-(3-benzyloxyphenyl)propyl]-1H-1,2,3-triazole収率 37.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

In an argon atmosphere, 1H-1,2,3-triazole (0.9 g) was dissolved in DMF (20 ml); 65% oily sodium hydride (0.48 g) was added. After stirring for 30 minutes, a solution of benzyl 3-(3-iodopropyl)phenyl ether (3.53 g) in DMF (5 ml) was added, followed by stirring at room temperature for 19 hours. The reaction mixture was diluted with ethyl acetate and washed with water and saturated saline. Under reduced pressure, the solvent was distilled off; the residue was subjected to column chromatography to yield the titled compound (1.1 g) as colorless crystals.

後処理

  1. stirringby stirring at room temperature for 19 hours
  2. washwashed with water and saturated saline
  3. distillationUnder reduced pressure, the solvent was distilled off

出典と根拠

ORDレコード
ord-97cbaffd525341eaaf687188f14621fc
出典データセット
uspto-grants-2004_04
特許番号
US06716863B2

反応ノート

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