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

HRID 2084376노트

반응식

HRID 2084376 반응식
[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

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 22733348Benzyl 3-(3-iodopropyl)phenyl etherHCID 178418936HCID 178418936, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-97cbaffd525341eaaf687188f14621fc
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716863B2

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