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Tin atom → 3-Amino-6-methoxy-2-[(phenylsulfonyl)methyl]-pyridine

HRID 731571
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인쇄 미리보기

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HRID 731571 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH2:9][S:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)(=[O:12])=[O:11])[C:6]([N+:19]([O-])=O)=[CH:5][CH:4]=1.[Sn]>CO.Cl>[NH2:19][C:6]1[C:7]([CH2:9][S:10]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)(=[O:12])=[O:11])=[N:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5352426Tin atomHCID 13902761(6-Methoxy-3-nitro-2-pyridinyl)methyl phenyl sulfone

생성물 1

HCID 220281923-Amino-6-methoxy-2-[(phenylsulfonyl)methyl]-pyridine수율 94.5%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

A stirred mixture of 6-methoxy-3-nitro-2-[(phenylsulfonyl)methyl]-pyridine (6.17 g, 20.0 mmol) in methanol and concentrated HCl (50 mL) is treated with thin strips of tin foil (10.0 g, 84.2 mmol), heated at 60° C. for 20 h, and filtered hot. The filtrate is poured over ice and 2.5N aqueous NaOH, stirred for 0.5 h and filtered. The filtercake is air-dried to afford the title compound as a white solid 5.26 g (94% yield), identified by mass spectral and HNMR analyses.

후처리

  1. filtrationfiltered hot
  2. additionThe filtrate is poured over ice and 2.5N aqueous NaOH
  3. filtrationfiltered
  4. customThe filtercake is air-dried

출처 및 근거

ORD 기록
ord-f9244049e53f474eb0ebf5bad34cbe87
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585873B2

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