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Thionyl Chloride → HCID 21913155, 화합물

HRID 1008073
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HRID 1008073 반응식
S(Cl)([Cl:3])=O.[CH3:5][C:6]1[C:11]([CH3:12])=[C:10]([NH:13][CH2:14][CH2:15][CH2:16]O)[C:9]([N+:18]([O-:20])=[O:19])=[C:8]([O:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:7]=1>ClCCl>[ClH:3].[Cl:3][CH2:16][CH2:15][CH2:14][NH:13][C:10]1[C:9]([N+:18]([O-:20])=[O:19])=[C:8]([O:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:7]=[C:6]([CH3:5])[C:11]=1[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 21913299HCID 21913299, 화합물

생성물 1

HCID 21913155HCID 21913155, 화합물수율 187%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Thionyl chloride (2.86 mL, 39.2 mmol) was added to a chilled (0° C.) solution of 3-[(2,3-dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]propan-1-ol (11.3 g, 35.6 mmol) in dichloromethane (170 mL). The reaction mixture was stirred at ambient temperature for 0.5 hr and then heated at reflux for 0.5 hr. The reaction mixture was allowed to cool to ambient temperature. A precipitate was isolated by filtration and then dried under vacuum to provide 13.64 g of N-(3-chloropropyl)-2,3-dimethyl-5-nitro-6-phenoxypyridin-4-amine hydrochloride.

후처리

  1. temperatureheated
  2. temperatureat reflux for 0.5 hr
  3. temperatureto cool to ambient temperature
  4. customA precipitate was isolated by filtration
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-307a80884b0341d5ab385a8702c85354
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06797718B2

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