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Sodium Azide → 4-[3-azidomethyl-5-(3,5-dichlorophenylthio)-1-isopropyl-1H-pyrazol-4-ylmethyl]pyridine

HRID 1862470
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HRID 1862470 반응식
Cl.Cl[CH2:3][C:4]1[C:8]([CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[C:7]([S:16][C:17]2[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[CH:18]=2)[N:6]([CH:25]([CH3:27])[CH3:26])[N:5]=1.[N-:28]=[N+:29]=[N-:30].[Na+]>CN(C)C=O>[N:28]([CH2:3][C:4]1[C:8]([CH2:9][C:10]2[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=2)=[C:7]([S:16][C:17]2[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[CH:18]=2)[N:6]([CH:25]([CH3:27])[CH3:26])[N:5]=1)=[N+:29]=[N-:30]
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참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 693533844-[3-chloromethyl-5-(3,5-dichlorophenylthio)-1-isopropyl-1H-pyrazol-4-ylmethyl]pyridine hydrochloride

생성물 1

HCID 867588894-[3-azidomethyl-5-(3,5-dichlorophenylthio)-1-isopropyl-1H-pyrazol-4-ylmethyl]pyridine수율 106.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 120 mg of 4-[3-chloromethyl-5-(3,5-dichlorophenylthio)-1-isopropyl-1H-pyrazol-4-ylmethyl]pyridine hydrochloride in 1 ml of anhydrous dimethylformamide stirred at room temperature was added 85 mg of sodium azide. The mixture was stirred for 1 h. The mixture was partitioned between diethyl ether and water then extracted three times. The combined extracts were reduced under reduced pressure to give 120 mg of 4-[3-azidomethyl-5-(3,5-dichlorophenylthio)-1-isopropyl-1H-pyrazol-4-ylmethyl]pyridine as a yellow oil which was used without any further purification. Mass spectrum (ESI) 433 [M+H]+.

후처리

  1. customThe mixture was partitioned between diethyl ether and water
  2. extractionthen extracted three times

출처 및 근거

ORD 기록
ord-2a751e8190c24792926f53898040f713
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06538015B1

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